CN109423331A - A kind of separation system and its separation method of petroleum Group Component - Google Patents
A kind of separation system and its separation method of petroleum Group Component Download PDFInfo
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- CN109423331A CN109423331A CN201710778479.5A CN201710778479A CN109423331A CN 109423331 A CN109423331 A CN 109423331A CN 201710778479 A CN201710778479 A CN 201710778479A CN 109423331 A CN109423331 A CN 109423331A
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- 238000000926 separation method Methods 0.000 title claims abstract description 135
- 239000003208 petroleum Substances 0.000 title claims abstract description 71
- 239000002904 solvent Substances 0.000 claims abstract description 207
- 238000001179 sorption measurement Methods 0.000 claims abstract description 131
- 238000001816 cooling Methods 0.000 claims abstract description 86
- 239000000463 material Substances 0.000 claims abstract description 32
- 238000007664 blowing Methods 0.000 claims abstract description 18
- 230000008676 import Effects 0.000 claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims description 85
- 239000007788 liquid Substances 0.000 claims description 82
- 230000008020 evaporation Effects 0.000 claims description 80
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 69
- 238000004090 dissolution Methods 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- 238000003795 desorption Methods 0.000 claims description 44
- 239000003205 fragrance Substances 0.000 claims description 39
- 239000000084 colloidal system Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 238000005259 measurement Methods 0.000 claims description 17
- 238000000605 extraction Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 239000002808 molecular sieve Substances 0.000 claims description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000002250 absorbent Substances 0.000 claims description 9
- 230000002745 absorbent Effects 0.000 claims description 9
- 239000002156 adsorbate Substances 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 238000000638 solvent extraction Methods 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011552 falling film Substances 0.000 claims description 3
- 239000003456 ion exchange resin Substances 0.000 claims description 3
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005191 phase separation Methods 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000010779 crude oil Substances 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 4
- 238000002203 pretreatment Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 24
- 239000000047 product Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 238000004587 chromatography analysis Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 238000001944 continuous distillation Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
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- 238000005119 centrifugation Methods 0.000 description 1
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- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000000921 elemental analysis Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1077—Vacuum residues
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention discloses the separation system and its separation method of a kind of petroleum Group Component.First adsorption tower top exit of the separation system is sequentially connected with the first evaporator, the first cooling tank, rectifying column, and the first adsorption tower outlet at bottom is connected with the material inlet of the second adsorption tower lower part, and the first adsorption tower top is additionally provided with the first steam blowing import；Second adsorption tower top exit is sequentially connected with the second evaporator, the second cooling tank, rectifying column, second adsorption tower outlet at bottom is sequentially connected with third cooling tank, third evaporator, extractor, rectifying column, and the second adsorption tower top is additionally provided with the second steam blowing import；Third evaporator is additionally provided with the entrance of third solvent, and extractor is additionally provided with the entrance of the 4th solvent.The system is continuous, carries out Group component separation to crude oil sample to a large amount of, high-purity, low solvent consumption, realizes the recycling of solvent, can continuously separate multiple samples, does not have to pre-treatment step.
Description
Technical field
The present invention relates to the separation systems and its separation method of a kind of petroleum Group Component.
Background technique
Hydrocarbon molecules isomer is more in petroleum, so even being apparent molecular weight, the similar two kinds of petroleum of boiling range
The product oil of sample, purification often has biggish difference.Generally for the structure composition feature of intuitive reflection petroleum, with hydrocarbon
Petroleum is divided into four races as partitioning standards and formed by class Group Component, respectively saturation point, fragrance point, resin and asphalt.
By the comparison and analysis to the ethnic constituent content of different oil products four, petroleum composition structure can be fast and accurately demarcated.
Conventional petroleum Group Component measuring method needs to be dissolved, filtered using normal heptane, toluene, ethyl alcohol and chromatographic column
And absorption, specific steps include: that sample is settled out asphalitine with normal heptane, after filtering, are flowed back and are removed in precipitating with normal heptane
The solvable point being mingled with, again with toluene reflux dissolution precipitating, obtain asphalitine.By deasphalting partial adsorbates in an aluminium oxide color
It composes on column, is successively unfolded and washes out chromatography on alumina column, chromatography on alumina column with normal heptane (petroleum ether), toluene, toluene-ethano
It is as shown in Figure 1 that lower section successively obtains saturation point, fragrance point and colloid, detailed process.
But the above method has the following problems:
(1) usually dissolution needs to handle 1g oil product sample using the solvent of 50~100g every time, and process needs are a large amount of
Manual operation, therefore be only capable of measurement four kinds of Group Components content, can not largely separate, prepare four kinds of Group Components.In crude oil
During characterization, usually to the saturation of wherein lightweight point and fragrance grouping point, it usually needs carry out BMCI value characterization, boiling range is surveyed
The experiments such as the measurements such as fixed, the latent value of virtue；For the asphalitine of complicated composition, in order to convert impurity composition therein, need accurately to survey
The aromatic ring of fixed wherein condensed-nuclei aromatics constitutes distribution, macromolecule hydrocarbon structure distribution feature.The above calibration process is required to largely
Group Component sample, it usually needs the raw material of 100~500g or more will consume 100~500 times of solvents using conventional separation methods.
Therefore, according to conventional method elution, prepare these samples, not only need a large amount of solvent, at the same also need hundreds of hours into
Row experimental implementation, risk is very big, reliability is extremely low；
(2) since last time tests remaining ethyl alcohol, toluene solvant will affect the saturation in next normal heptane point, fragrance point and colloid
Etc. components solubility, and separate after ethyl alcohol also into saturation point, fragrance point, toluene enter saturation point etc., cause final group
Divide assay inaccuracy.Therefore, existing method requires to remake chromatographic column before measure next time.But existing point
Analysis method carries out test to 1g oil product sample and needs using 40g chromatograph packing material, if carrying out to the raw material for needing 100~500g or more
When processing, then it is generally necessary to which 100~500 times of fillers, a large amount of filler cause very expensive testing cost, need in addition big
The solvent of amount and hundreds of hours are operated, cause existing analysis method be difficult low cost, high efficiency extract 100~500g with
On Group Component sample；
(3) if reusing chromatographic column normal heptane-miscible system of ethyl alcohol-sample also occurs, or even it will appear normal heptane-first
Benzene-miscible the system of ethyl alcohol-sample；There are also existing analysis methods during separation saturation point, fragrance point and colloid, Duo Zhongrong
Agent is successively repeatedly eluted, and will appear the miscible solvent of diversified forms in the component isolated, and but also to use first
The mixed solvents such as benzene-ethyl alcohol, but existing method for recovering solvents is difficult the miscible solvent of above-mentioned diversified forms carrying out high-purity
Ground separation causes spent solvent can not achieve and realizes recycling again, causes the discarded waste of solvent, with high costs；
(4) phenomena such as use of multi-solvents can also make saturation point raw miscible with fragrance distribution.
Therefore, existing analysis method, chromatographic column are repeatedly used has mutually punching between recycled solvent three
Prominent relationship causes existing analysis method to be difficult the Group Component sample that inexpensive, high efficiency extracts 100~500g or more.
101644698 A of patent CN provides a kind of chromatography of rodlike thin layer of crude oil SARA family component.This method passes through
Solvent dissolves and carries out chromatography, can measure the content of Group Component in crude oil, however lacks continuous Preparation equipment and separation
Equipment can not handle the crude oil sample of 10g or more and isolated each Group Component.
204188437 U of patent CN provides in a kind of rock organic solvent point in soluble organic and petroleum Group Component
From device.The device can make to evaporate solvent by concatenated water-bath and evaporation panel, and the Group Component under remaining is as product.
This method addresses only colloid, the slower problem of solvent evaporation rate in asphalitine purification process, but can not separate it is not of the same clan
Multi-solvents are added when component respectively and implement separation；Further, since solvent volatilization process is not provided with circular regeneration equipment, work as system
The safe and environment-friendly problem of solvent volatilization can not ensure when standby a large amount of samples.
101070495 B of patent CN describes a kind of mildization coal-family component separation method based on extraction with back extraction,
Its main feature is that repeatedly extraction, back extraction, distillation, washing process are used in series.However this method is suitable for the coals quality such as raw coal
Separation, and due to the presence of extracting process, it is necessary to while two kinds of solvents are used, when handling petroleum, the use of multi-solvent will make
Saturation point and fragrance distribution life are miscible, and what colloid also can be different degrees of be dissolved in two kinds of solvents, cause isolated saturation divide and
Fragrant sub-prime amount composition measuring result substantial deviation is practical, is not used to petroleum Group component separation and measurement.
At present do not have been reported that method can with low solvent consumption, safely and fast, the reusable petroleum race group of chromatographic column
The separation method divided.
Summary of the invention
In view of the deficiencies in the prior art, the present invention provides the present invention provides a kind of separation system of petroleum Group Component and
Its separation method.The system is continuous, the purpose of Group component separation is carried out to a large amount of, high-purity, low solvent consumption to crude oil sample,
It realizes the recycling of continuous operation, automatic production and solvent, and after completing a sample separation, can carry out at once next
The separation of sample does not have to carry out pre-treatment step (washing and replacement adsorption tower etc.).
The present invention provides a kind of separation system of petroleum Group Component comprising the first adsorption tower, the second adsorption tower, first are steamed
Send out device, the second evaporator, third evaporator, extractor, rectifying column, the first cooling tank, the second cooling tank and third cooling tank；
First adsorption tower is the adsorption tower for adsorption and desorption fragrance point and colloid, and first at the top of the first adsorption tower is unadsorbed
Object outlet be sequentially connected with the first evaporator, the first cooling tank, rectifying column, first absorption tower bottom first desorption object outlet and
The material inlet of second adsorption tower lower part is connected, and the first adsorption tower top is additionally provided with the first steam blowing import；Preferably,
The first unadsorbed object outlet at the top of one adsorption tower is connected with the entrance of the first evaporator, the evaporation solvent outlet of the first evaporator
It is connected with the import of the first cooling tank, the supernatant liquid outlet of the first cooling tank is connected with the entrance of rectifying column；
Second adsorption tower is adsorption tower for adsorption and desorption colloid, the unadsorbed object outlet of second at the top of the second adsorption tower with
Second evaporator, the second cooling tank, rectifying column are sequentially connected；Preferably, the second unadsorbed object outlet at the top of the second adsorption tower
It is connected with the entrance of the second evaporator, the evaporation solvent outlet of the second evaporator is connected with the import of the second cooling tank, and second is cold
But the supernatant liquid outlet of tank is connected with the entrance of rectifying column；
Second desorption object outlet of the second absorption tower bottom and third cooling tank, third evaporator, extractor, rectifying column successively phase
Even, it is preferable that second absorption tower bottom second desorption object outlet is connected with the import of third cooling tank, third cooling tank it is upper
Layer liquid outlet is connected with the entrance of third evaporator, and the evaporation solvent outlet of third evaporator is connected with the entrance of extractor,
The supernatant liquid outlet of extractor is connected with rectifying column；
Second adsorption tower top is additionally provided with the second steam blowing import；
Third evaporator is additionally provided with the entrance of third solvent, and extractor is additionally provided with the entrance of the 4th solvent.
Separation system further includes the first elutriator and the second elutriator；
First elutriator, for extracting the soluble matter of petroleum by the dissolution of the first solvent and isolating insoluble matter, first is washed
First elution taphole of de- device is connected with the material inlet of the first adsorption tower, the insoluble matter outlet and second of the first elutriator
Elutriator entrance is connected；Preferably, the entrance of the first elutriator is connected with petroleum supply pipeline；
Second elutriator, for isolating the solution dissolved with asphalitine by the asphalitine in the second solvent dissolution insoluble matter,
Preferably, the asphalitine outlet of the second elutriator is connected with asphalitine collection device.
First elutriator is provided with the first mixed dissolution unit, the first solid-liquid separation unit and the first heating unit, and first
The outlet of mixed dissolution unit is connected with the entrance of the first solid-liquid separation unit, the liquid outlet of the first solid-liquid separation unit and
The entrance of one adsorption tower is connected, and solid-phase outlet is connected with the entrance of the second elutriator；First heating unit is used for first
Dissolution kettle and the first drum filter are heated；Preferably, the first mixed dissolution unit includes the first dissolution kettle, described
First solid-liquid separation unit includes the first drum filter；
Second elutriator is provided with the second mixed dissolution unit, the second solid-liquid separation unit and the second heating unit, the second mixing
Dissolution unit outlet be connected with the entrance of the second solid-liquid separation unit, second heating unit for the second dissolution kettle with
Second drum filter is heated；Preferably, the second mixed dissolution unit includes the second dissolution kettle, second solid-liquid
Separative unit includes the second drum filter.
Circulation pipe is also connected between the entrance of first solid-liquid separation unit and the liquid outlet of the first solid-liquid separation unit
Line is provided with valve body on pipeloop.
The top exit of the rectifying column is also connected with the entrance of the first elutriator；Rectifier bottoms outlet is also washed with second
The entrance of de- device is connected.
First elutriator is provided with the first evaporation element, the entrance and the first solid-liquid separation unit of first evaporation element
Liquid outlet be connected, the vapor outlet port of first evaporation element is connected with rectifying column inlet；
Second elutriator is provided with the second evaporation element, the entrance of second evaporation element and the liquid of the second solid-liquid separation unit
Body outlet is connected, and the vapor outlet port of second evaporation element is connected with rectifying column inlet.
First evaporator is evaporator for evaporate the first solvent, and the second evaporator is for the first solvent of evaporation and the
The evaporator of two solvents, third evaporator are the evaporator for evaporating the second solvent and third solvent；Preferably, the first evaporation
The evaporation excess of device bottom is exported divides collection device to be connected with saturation, the outlet of evaporation excess and the fragrance point of the second base of evaporator
Collection device is connected, and the evaporation excess outlet of third base of evaporator is connected with colloid collection device；It is further preferred that first
Evaporator, the second evaporator and third evaporator use single-action or multiple-effect falling film evaporator.
Extractor is for being separated by extraction the second solvent and third solvent, it is preferable that the bottom solution of extractor exports
It is connected with solvent slop collection device, it is further preferred that extractor is using material filling type extractor, rotating disc type extractor or centrifugation extraction
Take device.
First solvent is one of normal heptane, n-hexane, petroleum ether；Second solvent includes one of toluene, benzene；The
Three solvents are one of ethyl alcohol, methanol, propyl alcohol；4th solvent is water.
First adsorption tower and the second adsorption tower are filling adsorption tower, and aluminium oxide, 5A molecular sieve, silicon are wherein filled in tower
It is one or more of in glue, macroporous absorbent resin and ion exchange resin；Preferably, macroporous absorption tree is filled in the first adsorption tower
Rouge, 5A molecular sieve and alumina packing are filled with macroporous absorbent resin, 5A molecular sieve and silica filler in the second adsorption tower.
First cooling tank, the second cooling tank and third cooling tank are respectively used to separate water in material, it is preferable that first is cooling
Tank, the bottom of the second cooling tank and third cooling tank, middle part are respectively arranged with water outlet and oily outlet.
Rectifying column is the rectifying column for the first solvent, the second solvent two component continuous distillation, it is preferable that rectifying column uses
Multistage rectifying column, the top exit of rectifying column are the outlet of low-boiling first solvent, and the outlet at bottom of rectifying column is high boiling
The outlet of second solvent of point is it is further preferred that the side line of rectifying column is provided with the outlet of impurity solvent.
The top exit of rectifying column is connected with the first colvent inlet of top of the first adsorption tower；The outlet at bottom of rectifying column with
The second material entrance of the lower part of second adsorption tower is connected with second colvent inlet on top.
The 4th cooling tank is additionally provided on the pipeline that the first adsorption tower is connect with the second adsorption tower, the 4th cooling tank is used for
Water in separation of material, it is preferable that bottom, the middle part of the 4th cooling tank are respectively arranged with water outlet and oily outlet.
The present invention provides a kind of separation methods of petroleum Group Component, are carried out using above-mentioned separation system to petroleum
The separation of petroleum Group Component.
Separation method includes the following steps:
With the saturation in the first solvent extraction petroleum point, fragrance point and colloid, extracting solution is obtained；
Extracting solution enters Ta Nei from the material inlet of the first adsorption tower lower part and adsorbs, the first unadsorbed solvent and full
The first evaporator is entered by the first unadsorbed object outlet with point, then evaporates the first evaporant containing the first solvent, the
One evaporant enters the first cooling tank and is cooled down and water vapour is made to be condensed into liquid water, thus and separation of oil, first is cooling
Oil in tank mutually enters rectifying column and carries out rectifying, while obtaining saturation point in the first base of evaporator；After the completion of absorption, steam from
First steam blowing import enters the first adsorption tower, carries out reverse blow, desorption to the first adsorbate in the first adsorption tower, obtains
To the first desorption mixture；
First desorption mixture is mixed with the second solvent, then enters the second adsorption tower from the material inlet of the second adsorption tower lower part
And it adsorbs；Unadsorbed the first solvent, the second solvent and fragrance point enter the second evaporator, then evaporate and contain the
Second evaporant of one solvent and the second solvent, the second evaporant enter the second cooling tank and are cooled down and be condensed into water vapour
Liquid water, thus and separation of oil；Oil in second cooling tank mutually enters rectifying column and carries out rectifying, while in the second evaporator bottom
Portion obtains fragrance point；After the completion of absorption, steam enters the second adsorption tower from the second steam blowing import, in the second adsorption tower
Second adsorbate carries out reverse blow, desorption, obtains the second desorption mixture；
Second desorption mixture enters third cooling tank and is cooled down and water vapour is made to be condensed into liquid water, to make water and oily phase
Separation；Oil in third cooling tank mutually enters third evaporator, then evaporates the third containing the second solvent and third solvent
Evaporant is extracted subsequently into extractor, while obtaining colloid in third base of evaporator；Wherein, in third cooling tank
During or after interior oil mutually enters third evaporator, third evaporator inlet is also passed through third solvent；
Before third evaporant enters extraction process, in or after the process, extractor entrance is also passed through the 4th solvent and is extracted；
After the completion of extractor, the rectifying column that enters that the extract liquor of the second solvent is contained on extractor top carries out rectifying.
With in the first solvent extraction petroleum saturation point, fragrance point and colloid specific steps are as follows: petroleum with
The first solvent that fresh the first solvent and/or rectifying column rectifying obtains is added to together in the first elutriator, and then first is mixed
It closes dissolution and first to be separated by solid-liquid separation, obtains insoluble matter and extracting solution；Preferably, the temperature of the first mixed dissolution is 25~90 DEG C,
Time is 5~30min, and the first temperature being separated by solid-liquid separation is 25~90 DEG C, and the time is 1~10min；
Insoluble matter is discharged into the second elutriator again, while being passed through the second solvent to the second elutriator, then the second mixed dissolution and
Second is separated by solid-liquid separation, and obtains the second solvent solution dissolved with asphalitine；Preferably, the temperature of the second mixed dissolution be 25~
110 DEG C, the time is 5~30min, and the second temperature being separated by solid-liquid separation is 25~110 DEG C, and the time is 1~10min.
When the first elutriator is provided with the first evaporation element, after the separation of solid and liquid of carry out first, extracting solution is first emitted into
First evaporation element, the first evaporation element are evaporated concentration to extracting solution, and the extracting solution after concentration is then emitted into first
Adsorption tower, the evaporation gas phase of the first evaporation element, which is emitted into rectifying column, carries out rectifying；
When the second elutriator is provided with the second evaporation element, carry out second separation of solid and liquid after, dissolved with asphalitine second
Solvent solution is first emitted into the second evaporation element, and first the second solvent solution of evaporation element is evaporated concentration, and the second evaporation is single
The evaporation gas phase of member, which is emitted into rectifying column, carries out rectifying；
It is added to petroleum in the first elutriator, the weight ratio of the first fresh solvent is 1:(0~5), it is added to the
The weight ratio of petroleum, the second fresh solvent in two elutriators is 1:(0~3).
The adsorption temp of first adsorption tower is 20~40 DEG C, and the desorption temperature of steam blowing is 100~158 DEG C；Second inhales
20~40 DEG C of the adsorption temp of attached tower, the desorption temperature of steam blowing are 100~158 DEG C.
The temperature that first evaporator is evaporated is 100~105 DEG C；The temperature that second evaporator is evaporated is 105.0
~110.6 DEG C；The temperature that third evaporator is evaporated is 105.0~110.6 DEG C；Quantity of solvent is less than 1% in evaporated residue.
The weight ratio of petroleum and third solvent, the 4th solvent is 1:(0~2): (10~100).
Separation method further include: the saturation of the first base of evaporator point is emitted into saturation and divides collection device, the second evaporator
The fragrance of bottom point is emitted into fragrance and divides collection device, and the colloid of third base of evaporator is emitted into colloid collection device.
Separation method further include: the side line of rectifying column, which is drawn, removes the solution containing impurity.
Petroleum can be the hydrocarbon raw material containing four components, such as crude oil, straight-run gas oil, wax tailings, pitch, normal pressure
Residual oil and decompression residuum etc..
Compared with prior art, the separation system of petroleum Group Component of the invention has the beneficial effect that:
(1) separation system of petroleum Group Component of the invention is connected using two adsorption towers, one of absorption and the first evaporation
Device, rectifying column are connected, and the second absorption is connected with the second evaporator, third evaporator, rectifying column, and extractor and third are evaporated
Device, rectifying column are connected, to constitute overall separation system, while dividing in separation process in saturation point, fragrance, reversed by steam
Purging is desorbed, and the second solvent (toluene), third solvent (ethyl alcohol) also is added in proper moment, and pass through cooling tank point
Water is separated out, there are also extraction process to introduce the not used novel solvent water of conventional method, and such technical solution integrally combines, from
And realize the reuse of adsorption tower, while can also be always ensured that only the first solvent (normal heptane), the second solvent (toluene)
Or both mixed liquor just can enter rectifying column, to realize the first solvent (normal heptane), the second solvent (toluene) high-purity point
From, achieve the purpose that recycling, and avoid toluene enter saturation point, ethyl alcohol enter saturation point and/or fragrance point, avoid out
Existing normal heptane-ethyl alcohol-sample, the normal heptane-miscible system of toluene-ethano-sample, it is final realize continuous, a large amount of, high-purity,
The purpose that Group component separation is carried out to low solvent consumption to crude oil sample realizes the circulation of continuous operation, automatic production and solvent
It uses, and after completing a sample separation, the separation of next sample can be carried out at once, do not have to progress pre-treatment step and (wash
Wash and replace adsorption tower etc.).
(2) separation system of petroleum Group Component of the invention is provided with the first elutriator and second and washes device, can will be in petroleum
Interval, the manual extraction process of asphalitine are improved to continuous operation, the preparation process that produces automatically, do not introduce chemical modification or
In the case that pitch increases production, the asphalitine Group Component that can be sufficiently reserved in former residual oil sample, and shadow is not caused to other Group Components
It rings, can guarantee the precise measurement to asphaltene in vacuum residues Group Component content while a large amount of continuous preparation asphalitines；Furthermore it can
Elution, filtering, a large amount of solvent flashings in evaporation process are sufficiently recycled, solvent consumption, the safety of lifting device are reduced
And reduce pollution.
(3) separation system of petroleum Group Component of the invention, the first elutriator and second wash device and are provided with evaporation element, can
It is concentrated with the toluene solvant to extracting solution and containing asphalitine, the extracting solution after concentration is conducive to improve it in the first absorption
The adsorption effect of tower and raising, the desorption effect of the first solvent (normal heptane) reverse blow.
(4) separation method of petroleum Group Component of the invention, for asphalitine and saturation point, fragrance point in a solvent molten
Solution degree difference is eluted repeatedly using multi-solvents, and is utilized respectively four kinds of Group Components in evaporation and adsorption tower separation petroleum, also
Using the first solvent of rectifying column circulation and stress and the second solvent, the ethnic constituent content of the four of preparation and actual value deviation are smaller,
Preparing product can be used for further accurate Characterization, and to solve, four kinds of Group Component preparation amounts are small in petroleum, solvent-oil ratio is big is asked
Topic.
Detailed description of the invention
Fig. 1 is the flow chart of the measuring method of existing slag oil asphalt matter component；
Fig. 2 is the schematic diagram of the separation system of the petroleum Group Component in an embodiment of the present invention；
Fig. 3 is the schematic diagram of the separation system of the petroleum Group Component in another embodiment of the present invention；
Appended drawing reference: the first elutriator of 1-；The second elutriator of 2-；The first adsorption tower of 3-；The second adsorption tower of 4-；5- first evaporates
Device；The second evaporator of 6-；7- third evaporator；8- extractor；9- rectifying column；The first cooling tank of 10-；The second cooling tank of 11-；
12- third cooling tank；A- petroleum；The first solvent of B-；The second solvent of C-；The 4th solvent of D-；E- asphalitine；F- saturation point；
G- fragrance point；H- colloid；I- solvent slop；J- impurity；K- third solvent.
Specific embodiment
The separation system of petroleum Group Component of the invention, but it is not considered that the present invention are further illustrated below by attached drawing
It is limited only in the following embodiments and the accompanying drawings.
As shown in Fig. 2, the separation system of petroleum Group Component of the present invention, including the first adsorption tower 3, the second adsorption tower 4, first
Evaporator 5, the second evaporator 6, third evaporator 7, extractor 8, rectifying column 9, the first cooling tank 10, the second cooling tank 11 and
Three cooling tanks 12；The first evaporator 5, the first cooling tank 10 are successively passed through in the unadsorbed object outlet of the first of first adsorption tower, 3 top
It is connected with the entrance of rectifying column 9, the material of the first desorption object outlet and 4 lower part of the second adsorption tower of 3 bottom of the first adsorption tower enters
Mouth is connected, and 3 top of the first adsorption tower is additionally provided with the first steam blowing import；The second unadsorbed object at 4 top of the second adsorption tower
Outlet is successively connected by the second evaporator 6, the second cooling tank 11 with the entrance of rectifying column 9, and the second of 4 bottom of the second adsorption tower
The outlet of desorption object is connected by third cooling tank 12 with the entrance of third evaporator 7, and 4 top of the second adsorption tower is provided with the second steaming
Vapour purges import；Third evaporator 7 is provided with the entrance of third solvent, third evaporation outlet and the extractor 8 of third evaporator 7
Entrance is connected；Extractor 8 is provided with the entrance of the 4th solvent, and the top taphole of extractor 8 is connected with rectifying column 9.
In one embodiment of the invention, separation system further includes the first elutriator 1 and the second elutriator 2；First
Elutriator 1, for extracting the soluble matter of petroleum A by the first solvent B dissolution and isolating insoluble matter, the first elutriator 1
The first elution taphole be connected with the material inlet of the first adsorption tower 3, the insoluble matter of the first elutriator 1 is exported and is washed with second
De- 2 entrance of device is connected；Preferably, the entrance of the first elutriator 1 is connected with petroleum A supply pipeline；Second elutriator 2 is used
In dissolving the asphalitine in insoluble matter by the second solvent C, the solution dissolved with asphalitine is isolated to get asphalitine E is arrived.It is excellent
The asphalitine outlet of selection of land, the second elutriator 2 is connected with asphalitine collection device.
First elutriator is provided with the first mixed dissolution unit, the first solid-liquid separation unit and the first heating unit, and first
The outlet of mixed dissolution unit is connected with the entrance of the first solid-liquid separation unit, the liquid outlet of the first solid-liquid separation unit and
The entrance of one adsorption tower 3 is connected, and solid-phase outlet is connected with the entrance of the second elutriator 2；First heating unit is used for the
One dissolution kettle and the first drum filter are heated；Preferably, the first mixed dissolution unit includes the first dissolution kettle, institute
Stating the first solid-liquid separation unit includes the first drum filter；Second elutriator 2 is provided with the second mixed dissolution unit, second solid
The outlet of liquid separative unit and the second heating unit, the second mixed dissolution unit is connected with the entrance of the second solid-liquid separation unit,
The second mixed dissolution unit preferably includes the second dissolution kettle, and second solid-liquid separation unit preferably includes second turn
Cylinder filter, second heating unit is for heating the second dissolution kettle and the second drum filter.
Circulation pipe is also connected between the entrance of first solid-liquid separation unit and the liquid outlet of the first solid-liquid separation unit
Line is provided with valve body on pipeloop.
The top exit of the rectifying column 9 is also connected with the entrance of the first elutriator 1；9 outlet at bottom of rectifying column is also with
The entrance of two elutriators 2 is connected.
First elutriator 1 is provided with the first evaporation element, and the entrance of first evaporation element and first are separated by solid-liquid separation single
The liquid outlet of member is connected, and the vapor outlet port of first evaporation element is connected with the entrance of rectifying column 9；Second elutriator 2 is set
It is equipped with the second evaporation element, the entrance of second evaporation element is connected with the liquid outlet of the second solid-liquid separation unit, described
The vapor outlet port of second evaporation element is connected with the entrance of rectifying column 9.
First evaporator 5 is evaporator for evaporate the first solvent, the second evaporator 6 be for evaporate the first solvent with
The evaporator of second solvent, third evaporator 7 are the evaporator for evaporating the second solvent and third solvent；Preferably, first
The evaporation excess of 5 bottom of evaporator is exported divides collection device to be connected with saturation, the evaporation excess of 6 bottom of the second evaporator export and
Fragrance divides collection device to be connected, and the evaporation excess outlet of 7 bottom of third evaporator is connected with colloid collection device；Further preferably
Ground, the first evaporator 5, the second evaporator 6 and third evaporator 7 use single-action or multiple-effect falling film evaporator.
Extractor 8 is for being separated by extraction the second solvent and third solvent, it is preferable that the bottom solution of extractor 8 goes out
Mouthful discharge solvent slop I, extractor 8 bottom solution outlet with solvent slop collection device be connected, then carry out third solvent again
It is separated with third solvent.It is further preferred that extractor 8 is using material filling type extractor, rotating disc type extractor or centrifugal extractor.
First solvent B includes one of normal heptane, n-hexane, petroleum ether；Second solvent C includes toluene, one in benzene
Kind；Third solvent includes one of ethyl alcohol, methanol, propyl alcohol；4th solvent is water.
First adsorption tower 3 and the second adsorption tower 4 are filling adsorption tower, and aluminium oxide, 5A molecular sieve, silicon are wherein filled in tower
It is one or more of in glue, macroporous absorbent resin and ion exchange resin, macroporous absorption tree is filled in preferably the first adsorption tower 3
Rouge, 5A molecular sieve and alumina packing are filled with macroporous absorbent resin, 5A molecular sieve and silica filler in the second adsorption tower 4.
First cooling tank 10, the second cooling tank 11 and third cooling tank 12 are respectively used to separate water in material, it is preferable that the
Bottom, the middle part of one cooling tank 10, the second cooling tank 11 and third cooling tank 12 are respectively arranged with water outlet and oily outlet.
Rectifying column 9 is the rectifying column for the first solvent, the second solvent two component continuous distillation, it is preferable that rectifying column 9 is adopted
With multistage rectifying column, the top exit of rectifying column 9 is the outlet of low-boiling first solvent, and the outlet at bottom of rectifying column 9 is
The outlet of high boiling second solvent leads to it is further preferred that the side line of rectifying column 9 is provided with the outlet of impurity solvent
Cross the impurity J that this outlet can be discharged in rectifying column.
In another embodiment of the invention, it is additionally provided on the pipeline that the first adsorption tower is connect with the second adsorption tower
4th cooling tank, the 4th cooling tank is for water in separation of material, it is preferable that bottom, the middle part of the 4th cooling tank are respectively arranged with
Water outlet and oily outlet.In this way, the desorption material of the first adsorption tower discharge is introduced into the 4th cooling tank, water and separation of oil
After enter back into the second adsorption tower.
In another embodiment of the invention, as shown in figure 3, the first solvent can also be used after the completion of steam blowing
Or second solvent carry out reverse blow, therefore, the first colvent inlet of top of the top exit of rectifying column 9 and the first adsorption tower 3
It is connected；The outlet at bottom of rectifying column 9 and the second material entrance of the lower part of the second adsorption tower 4 and the second colvent inlet phase on top
Even.
The present invention also provides the separation methods of the separation system based on petroleum Group Component, extract petroleum with the first solvent B
Saturation point, fragrance point and colloid in raw material A, obtain extracting solution；Extracting solution enters from the material inlet of 3 lower part of the first adsorption tower
It in tower and adsorbs, the first unadsorbed solvent B and saturation point pass through the first unadsorbed object outlet and enter the first evaporator
5, the first evaporant containing the first solvent B is then evaporated, the first evaporant enters the first cooling tank 10 and cooled down and made
Water vapour is condensed into liquid water, thus and separation of oil；The water of first cooling tank 10 discharge removes out-of-bounds recyclable device, and first is cooling
The oil that tank 10 is discharged mutually enters rectifying column 9 and carries out rectifying, while obtaining saturation in 5 bottom of the first evaporator and dividing F；Absorption is completed
Afterwards, steam L enters in the first adsorption tower 3, carries out reverse blow, desorption to the first adsorbate, obtains the first desorption mixture；
First desorption mixture is mixed with the second solvent, then enters the second absorption from the material inlet of 4 lower part of the second adsorption tower
Tower 4 simultaneously adsorbs；Unadsorbed the first solvent B, the second solvent C and fragrance point enter the by the second unadsorbed object outlet
Then two evaporators 6 evaporate the second evaporant containing the first solvent B and the second solvent C, it is cold that the second evaporant enters second
But tank 11 is cooled down and water vapour is made to be condensed into liquid water, thus and separation of oil；Shui Qu circle of second cooling tank 11 discharge
Outer recyclable device, the oil of the second cooling tank 11 discharge mutually enters rectifying column 9 and carries out rectifying, while obtaining in 6 bottom of the second evaporator
Divide G to fragrance；After the completion of absorption, steam L enters the second adsorption tower 4, carries out to the second adsorbate in the second adsorption tower 4 reversed
Purging, desorption, obtain the second desorption mixture；
Second desorption mixture enters third cooling tank 12 and is cooled down and water vapour is made to be condensed into liquid water, thus with oily phase point
From；The water that third cooling tank 12 is discharged removes out-of-bounds recyclable device, and the oil that third cooling tank 12 is discharged is mutually by from third evaporator 7
Entrance enters third evaporator 7, the third evaporant containing the second solvent and third solvent is then evaporated, subsequently into extraction
Device 8 is extracted, while obtaining colloid H in 7 bottom of third evaporator；Wherein, the oil in third cooling tank 12 mutually enters the
During or after three evaporators 7,7 entrance of third evaporator is also passed through third solvent；Enter extraction process in third evaporant
Before, in or after the process, 8 entrance of extractor is also passed through the 4th solvent D, and the 4th solvent D extracts third solvent；Extractor
After the completion of 8, the rectifying column 9 that enters that the extract liquor of the second solvent is contained on 8 top of extractor carries out rectifying.
Saturation point, the specific steps of fragrance point and colloid in petroleum A are extracted with the first solvent B are as follows: petroleum A
It is added in the first elutriator 1 together with the first solvent B that the first fresh solvent B and/or 9 rectifying of rectifying column are obtained, then
First mixed dissolution and first is separated by solid-liquid separation, and obtains insoluble matter and extracting solution；Preferably, the temperature of the first mixed dissolution be 25~
90 DEG C, the time is 5~30min, and the first temperature being separated by solid-liquid separation is 25~90 DEG C, and the time is 1~10min；Insoluble matter is arranged again
Enter the second elutriator 2, while being passed through the second solvent C to the second elutriator 2, then the second mixed dissolution and second is separated by solid-liquid separation,
Obtain the second solvent solution dissolved with asphalitine；Preferably, the temperature of the second mixed dissolution be 25~110 DEG C, the time be 5~
30min, the second temperature being separated by solid-liquid separation is 25~110 DEG C, and the time is 1~10min.
When the first elutriator 1 is provided with the first evaporation element, after the separation of solid and liquid of carry out first, extracting solution is first emitted into
First evaporation element, the first evaporation element are evaporated concentration to extracting solution, and the extracting solution after concentration is then emitted into first
Adsorption tower 3, the evaporation gas phase of the first evaporation element, which is emitted into rectifying column 9, carries out rectifying；When the second elutriator 2 is provided with second
When evaporation element, after the separation of solid and liquid of carry out second, the second solvent solution dissolved with asphalitine is first emitted into the second evaporation list
Member, first the second solvent solution of evaporation element are evaporated concentration, and the evaporation gas phase of the second evaporation element is emitted into rectifying column 9
Carry out rectifying；
It, can be with the of rectifying column rectifying when the first solvent of circulation, the second solvent are sufficient for the first elution and the second elution
One solvent, the second solvent are separately added into the first elutriator and the second elutriator.When internal circulating load deficiency, it is added to the first elutriator
The weight ratio of petroleum, the first fresh solvent in 1 can be 1:(0~5), the stone being added in the second elutriator 2
Oily raw material, the second fresh solvent weight ratio can be 1:(0~3).
The adsorption temp of first adsorption tower is 20~40 DEG C, and the desorption temperature of steam blowing is 100~158 DEG C；Second inhales
20~40 DEG C of the adsorption temp of attached tower, the desorption temperature of steam blowing are 100~158 DEG C.
The temperature that first evaporator 5 is evaporated is 100~105 DEG C；The temperature that second evaporator 6 is evaporated is
105.0~110.6 DEG C, the temperature that third evaporator 7 is evaporated is 105.0~110.6 DEG C.First evaporator, the second evaporation
When device and third evaporator are evaporated, saturation can be divided according to experiment, the requirement of fragrance point and colloid, solvent is steamed
Hair stops evaporation as when quantity of solvent is less than 1% in evaporated residue.
When not needing addition third solvent in third evaporator, the additive amount of third solvent can be 0.Petroleum and
Three solvents, the 4th solvent weight ratio be 1:(0~2): (10~100).
This method further include: the saturation of 5 bottom of the first evaporator point is emitted into saturation and divides collection device, the second evaporator 6
The fragrance of bottom point is emitted into fragrance and divides collection device, and the colloid of 7 bottom of third evaporator is emitted into colloid collection device.
This method further include: the side line of rectifying column 9, which is drawn, removes the solution containing impurity.
Embodiment 1
(1) first all devices of the present invention are normally driven to operate, 200 ~ 500kg that rectifying column obtains is added in the first elutriator 1
Normal heptane solvent, the second elutriator 2 the obtained 50 ~ 100kg toluene of rectifying column is added.By 0.5kg petroleum A1 and 0.1kg
The mixture of fresh normal heptane is added in the first elutriator 1, is then carried out the first mixed dissolution and first and is separated by solid-liquid separation, obtains
To extracting solution and insoluble matter；The temperature of first mixed dissolution is 85 DEG C, time 5min, and the first temperature being separated by solid-liquid separation is 85
DEG C, time 10min.
Extracting solution is first emitted into the first evaporation element, and the first evaporation element is evaporated concentration to extracting solution, then will be dense
Extracting solution after contracting is emitted into the first adsorption tower 3, the evaporation gas phase (normal heptane) of the first evaporation element be emitted into rectifying column 9 into
Row rectifying.
Insoluble matter is discharged into the second elutriator 2, while being passed through 0.1kg toluene to the second elutriator 2, it is mixed then to carry out second
It closes dissolution and second to be separated by solid-liquid separation, obtains the second solvent solution dissolved with asphalitine；The temperature of second mixed dissolution is 95 DEG C,
Time is 5min, and the second temperature being separated by solid-liquid separation is 95 DEG C, time 10min.After the separation of solid and liquid of carry out second, dissolved with drip
Second solvent solution of green matter is first emitted into the second evaporation element, and the second evaporation element is evaporated the second solvent solution dense
Contracting, the evaporation gas phase (toluene) of the second evaporation element, which is emitted into rectifying column 9, carries out rectifying.
(2) first extraction solution are filled with macroporous absorbent resin, 5A molecular sieve and alumina packing from the first adsorption tower 3()
The material inlet of lower part enters Ta Nei and adsorbs, and adsorption temp is 25 DEG C, and unadsorbed normal heptane and saturation point pass through
First unadsorbed object outlet enters the first evaporator 5, then evaporates normal heptane, is introduced into the first cooling tank 11 and is cooled down,
Steam is condensed into water and is layered with normal heptane, is discharged device from pot bottom, and upper layer normal heptane enters rectifying column 9 and carries out rectifying,
Saturation point is obtained in 5 bottom of the first evaporator simultaneously, or is further emitted into saturation and divides collection device；First evaporator 5 into
The temperature of row evaporation is 100~105 DEG C.
After the completion of the absorption of the first adsorption tower 3, the temperature of steam L(steam is 100 DEG C) enter the first adsorption tower 3, to the
The first adsorbate in one adsorption tower 3 carries out reverse blow, desorption, obtains the first desorption mixture.First desorption mixture is first
It mixes with toluene, is then emitted into the second adsorption tower 4 from the material inlet of 4 lower part of the second adsorption tower.
(3) first desorption mixtures are filled with macroporous absorbent resin, 5A molecular sieve and silica gel into the second adsorption tower 4(and fill out
Material) it adsorbs afterwards, adsorption temp is 25 DEG C, and unadsorbed normal heptane, toluene and fragrance point are gone out by the second unadsorbed object
Mouth enters the second evaporator 6, then evaporates the second evaporant containing normal heptane and toluene, the second evaporant is introduced into second
Cooling tank 10 is cooled down, and is condensed steam and is separated water outlet, and 10 middle part oil of cooling tank mutually enters rectifying column 9 and carries out rectifying, together
When 6 bottom of the second evaporator obtain fragrance point；The temperature that second evaporator 6 is evaporated is 105.0~110.6 DEG C.
After the completion of the absorption of second adsorption tower 4, the temperature of steam L(steam is 100 DEG C) enter the second adsorption tower 4, to second
The second adsorbate in adsorption tower 4 carries out reverse blow, desorption, obtains the second desorption mixture.Second desorption mixture is advanced
Enter third cooling tank and cooled down and separated water, then by entering third evaporator 7 from 7 entrance of third evaporator.
(4) after entering third evaporator 7, containing toluene and ethyl alcohol third evaporant is evaporated, subsequently into extractor 8
It is extracted, while obtaining colloid in 7 bottom of third evaporator, or colloid is further emitted into colloid collection device；Its
In, during the oil of third cooling tank mutually enters third evaporator 7, third evaporator inlet is also passed through ethyl alcohol, third evaporation
The temperature that device 7 is evaporated is 105.0~110.6 DEG C；Enter in extraction process in third evaporant, 8 entrance of extractor is also logical
Enter water, water extracts ethyl alcohol；After the completion of extractor 8,8 top of extractor extract liquor containing toluene enters rectifying column 9
Carry out rectifying.
Embodiment 2
The method of the present embodiment is substantially same as Example 1, and difference is: completing the four components separation of petroleum in embodiment 1
Afterwards, in holding meanss after existing solvent cycle operation 3h, switching another kind petroleum A2 continues the separation of four components.Work as institute
There is raw material to enter system and after being sufficiently separated, the no longer isolated new product of products export, by the normal heptane of rectifying column,
Toluene outlet switches to solvent storage device, and the operation of holding system is until all solvents are sufficiently recycled.Recovered solvent is available
In separation process next time.
The property of 1 petroleum of table
| Petroleum | A1 | A2 |
| Elemental analysis | ||
| C,% | 82.2 | 86.46 |
| H,% | 10.16 | 11.14 |
| S,% | 5.11 | 1.51 |
| N,ppm | 4193 | 3890 |
| Carbon residue, % | 23.91 | 12.71 |
| Molecular weight | 618 | 586 |
| The distillation of liquid High Temperature Simulation, % | ||
| IBP | 389.4 | 160.8 |
| 10% | 520.4 | 329 |
| 30% | 586.4 | 473 |
| 50% | 643.4 | 555.6 |
| 70% | 711.2 | 632.2 |
2 petroleum Group component separation result of table
| Standard method | Embodiment 1 | Standard method | Embodiment 2 | |
| Petroleum | A1 | A1 | A2 | A2 |
| Material quality, g | 1 | 500 | 1 | 500 |
| Normal heptane consumption, g | 150 | 500 | 200 | 200 |
| Toluene consumption, g | 200 | 700 | 200 | 300 |
| Unit Materials Solvents consumption, g/g | 350 | 2.4 | 400 | 1.0 |
| Measurement saturation point, % | 19.31 | 18.05 | 30.21 | 29.50 |
| Measurement fragrance point, % | 47.23 | 48.79 | 55.49 | 57.65 |
| Measure colloid, % | 27.91 | 27.05 | 12.87 | 12.86 |
| Measure asphalitine, % | 5.55 | 6.11 | 1.44 | 1.61 |
Note: standard method is tested by four compound mensuration method of NB SH/T 0509-2010 asphalt.
It should be noted that specific technical features described in the above specific embodiments, can pass through any conjunction
Suitable mode carries out any combination, equally fall into it is disclosed in this invention within the scope of.In addition, of the invention is a variety of different
Any combination can also be carried out between embodiment, as long as it does not violate the idea of the present invention, equally should be considered as the present invention
Disclosure of that.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited to above-mentioned realities
The detail in mode is applied, within the scope of the technical concept of the present invention, a variety of letters can be carried out to technical solution of the present invention
Monotropic type, these simple variants all belong to the scope of protection of the present invention.
Claims (24)
1. a kind of separation system of petroleum Group Component, which is characterized in that it includes the first adsorption tower, the second adsorption tower, the first steaming
Send out device, the second evaporator, third evaporator, extractor, rectifying column, the first cooling tank, the second cooling tank and third cooling tank；
First adsorption tower is the adsorption tower for adsorption and desorption fragrance point and colloid, and first at the top of the first adsorption tower is unadsorbed
Object outlet be sequentially connected with the first evaporator, the first cooling tank, rectifying column, first absorption tower bottom first desorption object outlet and
The material inlet of second adsorption tower lower part is connected, and the first adsorption tower top is additionally provided with the first steam blowing import；
Second adsorption tower is adsorption tower for adsorption and desorption colloid, the unadsorbed object outlet of second at the top of the second adsorption tower with
Second evaporator, the second cooling tank, rectifying column are sequentially connected, and the second desorption object outlet of the second absorption tower bottom and third are cooling
Tank, third evaporator, extractor, rectifying column are sequentially connected, and the second adsorption tower top is additionally provided with the second steam blowing import；
Third evaporator is additionally provided with the entrance of third solvent, and extractor is additionally provided with the entrance of the 4th solvent.
2. separation system according to claim 1, it is characterised in that: separation system further includes that the first elutriator and second are washed
De- device；
First elutriator, for extracting the soluble matter of petroleum by the dissolution of the first solvent and isolating insoluble matter, first is washed
First elution taphole of de- device is connected with the material inlet of the first adsorption tower, the insoluble matter outlet and second of the first elutriator
Elutriator entrance is connected；Preferably, the entrance of the first elutriator is connected with petroleum supply pipeline；
Second elutriator, for isolating the solution dissolved with asphalitine by the asphalitine in the second solvent dissolution insoluble matter,
Preferably, the asphalitine outlet of the second elutriator is connected with asphalitine collection device.
3. separation system according to claim 2, it is characterised in that: the first elutriator is provided with the first mixed dissolution list
Member, the first solid-liquid separation unit and the first heating unit, outlet and the first solid-liquid separation unit of the first mixed dissolution unit
Entrance is connected, and the liquid outlet of the first solid-liquid separation unit is connected with the entrance of the first adsorption tower, solid-phase outlet and the second elution
The entrance of device is connected；First heating unit is for heating the first dissolution kettle and the first drum filter；Preferably,
The first mixed dissolution unit includes the first dissolution kettle, and first solid-liquid separation unit includes the first drum filter；
Second elutriator is provided with the second mixed dissolution unit, the second solid-liquid separation unit and the second heating unit, the second mixing
Dissolution unit outlet be connected with the entrance of the second solid-liquid separation unit, second heating unit for the second dissolution kettle with
Second drum filter is heated；Preferably, the second mixed dissolution unit includes the second dissolution kettle, second solid-liquid
Separative unit includes the second drum filter.
4. measurement device according to claim 3, it is characterised in that: the entrance of the first solid-liquid separation unit and the first solid-liquid
It is also connected with pipeloop between the liquid outlet of separative unit, is provided with valve body on pipeloop.
5. the measurement device according to any one of claim 2-4, it is characterised in that: the top exit of the rectifying column
Also it is connected with the entrance of the first elutriator；Rectifier bottoms outlet is also connected with the entrance of the second elutriator.
6. measurement device according to claim 2, it is characterised in that: the first elutriator is provided with the first evaporation element, institute
The entrance for stating the first evaporation element is connected with the liquid outlet of the first solid-liquid separation unit, and the steam of first evaporation element goes out
Mouth is connected with rectifying column inlet；
Second elutriator is provided with the second evaporation element, the entrance of second evaporation element and the liquid of the second solid-liquid separation unit
Body outlet is connected, and the vapor outlet port of second evaporation element is connected with rectifying column inlet.
7. measurement device according to claim 1, it is characterised in that: the first evaporator is the steaming for evaporating the first solvent
Device is sent out, the second evaporator is the evaporator for evaporating the first solvent and the second solvent, and third evaporator is for evaporating second
The evaporator of solvent and third solvent；Preferably, the evaporation excess of the first base of evaporator, which is exported, divides collection device phase with saturation
Even, the evaporation excess of the second base of evaporator is exported divides collection device to be connected with fragrance, the evaporation excess of third base of evaporator
Outlet is connected with colloid collection device；It is further preferred that the first evaporator, the second evaporator and third evaporator use single-action
Or multiple-effect falling film evaporator.
8. measurement device according to claim 1, it is characterised in that: extractor for be separated by extraction the second solvent and
Third solvent, it is preferable that the bottom solution outlet of extractor is connected with solvent slop collection device, it is further preferred that extractor
Using material filling type extractor, rotating disc type extractor or centrifugal extractor.
9. measurement device according to claim 1, it is characterised in that: the first solvent is normal heptane, in n-hexane, petroleum ether
One kind；Second solvent includes one of toluene, benzene；Third solvent is one of ethyl alcohol, methanol, propyl alcohol；4th solvent
For water.
10. measurement device according to claim 1, it is characterised in that: the first adsorption tower and the second adsorption tower are that filler is inhaled
Attached tower is wherein filled in tower in aluminium oxide, 5A molecular sieve, silica gel, macroporous absorbent resin and ion exchange resin a kind of or several
Kind；Preferably, it is filled with macroporous absorbent resin, 5A molecular sieve and alumina packing in the first adsorption tower, is filled out in the second adsorption tower
Equipped with macroporous absorbent resin, 5A molecular sieve and silica filler.
11. measurement device according to claim 1, it is characterised in that: the first cooling tank, the second cooling tank and third are cooling
Tank is respectively used to separate water in material, it is preferable that the first cooling tank, the bottom of the second cooling tank and third cooling tank, middle part
It is not provided with water outlet and oily outlet.
12. measurement device according to claim 1, it is characterised in that: rectifying column is for the first solvent, the second solvent two
The rectifying column of component continuous rectification, it is preferable that rectifying column uses multistage rectifying column, and the top exit of rectifying column is low-boiling the
The outlet of one solvent, the outlet at bottom of rectifying column are the outlet of high boiling second solvent it is further preferred that rectifying column
Side line be provided with the outlet of impurity solvent.
13. measurement device according to claim 1, it is characterised in that: the top exit of rectifying column and the first adsorption tower
The first colvent inlet of top is connected；The second material entrance of the lower part of the outlet at bottom of rectifying column and the second adsorption tower and top
Second colvent inlet is connected.
14. measurement device according to claim 1, it is characterised in that: connect in the first adsorption tower with the second adsorption tower
The 4th cooling tank is additionally provided on pipeline, the 4th cooling tank is for water in separation of material, it is preferable that the bottom of the 4th cooling tank,
Middle part is respectively arranged with water outlet and oily outlet.
15. a kind of separation method of petroleum Group Component, it is characterised in that: using separation system described in claim 1-14 to stone
Oily raw material carries out the separation of petroleum Group Component.
16. separation method as claimed in claim 15, it is characterised in that: separation method includes the following steps:
With the saturation in the first solvent extraction petroleum point, fragrance point and colloid, extracting solution is obtained；
Extracting solution enters Ta Nei from the material inlet of the first adsorption tower lower part and adsorbs, the first unadsorbed solvent and full
The first evaporator is entered by the first unadsorbed object outlet with point, then evaporates the first evaporant containing the first solvent, the
One evaporant enters the first cooling tank and is cooled down and water vapour is made to be condensed into liquid water, thus and separation of oil, first is cooling
Oil in tank mutually enters rectifying column and carries out rectifying, while obtaining saturation point in the first base of evaporator；After the completion of absorption, steam from
First steam blowing import enters the first adsorption tower, carries out reverse blow, desorption to the first adsorbate in the first adsorption tower, obtains
To the first desorption mixture；
First desorption mixture is mixed with the second solvent, then enters the second adsorption tower from the material inlet of the second adsorption tower lower part
And it adsorbs；Unadsorbed the first solvent, the second solvent and fragrance point enter the second evaporator, then evaporate and contain the
Second evaporant of one solvent and the second solvent, the second evaporant enter the second cooling tank and are cooled down and be condensed into water vapour
Liquid water, thus and separation of oil；Oil in second cooling tank mutually enters rectifying column and carries out rectifying, while in the second evaporator bottom
Portion obtains fragrance point；After the completion of absorption, steam enters the second adsorption tower from the second steam blowing import, in the second adsorption tower
Second adsorbate carries out reverse blow, desorption, obtains the second desorption mixture；
Second desorption mixture enters third cooling tank and is cooled down and water vapour is made to be condensed into liquid water, to make water and oily phase
Separation；Oil in third cooling tank mutually enters third evaporator, then evaporates the third containing the second solvent and third solvent
Evaporant is extracted subsequently into extractor, while obtaining colloid in third base of evaporator；Wherein, in third cooling tank
During or after interior oil mutually enters third evaporator, third evaporator inlet is also passed through third solvent；
Before third evaporant enters extraction process, in or after the process, extractor entrance is also passed through the 4th solvent and is extracted；
After the completion of extractor, the rectifying column that enters that the extract liquor of the second solvent is contained on extractor top carries out rectifying.
17. separation method as claimed in claim 16, it is characterised in that: with the saturation in the first solvent extraction petroleum
Point, the specific steps of fragrance point and colloid are as follows: petroleum and the first fresh solvent and/or rectifying column rectifying obtain first
Solvent is added to together in the first elutriator, and then the first mixed dissolution and first is separated by solid-liquid separation, and obtains insoluble matter and extracting solution；
Preferably, the temperature of the first mixed dissolution is 25~90 DEG C, and the time is 5~30min, and the first temperature being separated by solid-liquid separation is 25~90
DEG C, the time is 1~10min；
Insoluble matter is discharged into the second elutriator again, while being passed through the second solvent to the second elutriator, then the second mixed dissolution and
Second is separated by solid-liquid separation, and obtains the second solvent solution dissolved with asphalitine；Preferably, the temperature of the second mixed dissolution be 25~
110 DEG C, the time is 5~30min, and the second temperature being separated by solid-liquid separation is 25~110 DEG C, and the time is 1~10min.
18. separation method as claimed in claim 16, it is characterised in that: when the first elutriator is provided with the first evaporation element
When, after the separation of solid and liquid of carry out first, extracting solution is first emitted into the first evaporation element, and the first evaporation element steams extracting solution
Hair concentration, is then emitted into the first adsorption tower for the extracting solution after concentration, the evaporation gas phase of the first evaporation element is emitted into rectifying
Rectifying is carried out in tower；
When the second elutriator is provided with the second evaporation element, carry out second separation of solid and liquid after, dissolved with asphalitine second
Solvent solution is first emitted into the second evaporation element, and first the second solvent solution of evaporation element is evaporated concentration, and the second evaporation is single
The evaporation gas phase of member, which is emitted into rectifying column, carries out rectifying.
19. separation method as claimed in claim 16, it is characterised in that: be added to petroleum in the first elutriator, new
The weight ratio of the first fresh solvent is 1:(0~5), it is added to the petroleum in the second elutriator, the second fresh solvent
Weight ratio be 1:(0~3).
20. separation method as claimed in claim 16, it is characterised in that: the adsorption temp of the first adsorption tower is 20~40 DEG C,
The desorption temperature of steam blowing is 100~158 DEG C；20~40 DEG C of the adsorption temp of second adsorption tower, the desorption temperature of steam blowing
Degree is 100~158 DEG C.
21. separation method as claimed in claim 16, it is characterised in that: the temperature that the first evaporator is evaporated be 100~
105℃；The temperature that second evaporator is evaporated is 105.0~110.6 DEG C；The temperature that third evaporator is evaporated is
105.0~110.6 DEG C；Quantity of solvent is less than 1% in evaporated residue.
22. separation method as claimed in claim 16, it is characterised in that: the weight of petroleum and third solvent, the 4th solvent
Amount ratio is 1:(0~2): (10~100).
23. separation method as claimed in claim 16, it is characterised in that: separation method further include: the first base of evaporator
Saturation point is emitted into saturation and divides collection device, and the fragrance point of the second base of evaporator is emitted into fragrance and divides collection device, and third is steamed
The colloid of hair device bottom is emitted into colloid collection device.
24. separation method as claimed in claim 16, it is characterised in that: separation method further include: the side line of rectifying column is drawn
Except the solution containing impurity.
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| CN110763644A (en) * | 2019-11-04 | 2020-02-07 | 长安大学 | A kind of separation method of asphalt four components |
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Effective date of registration: 20230906 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100020 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |