CN109423332A - A kind of separation system and its separation method of continuous separation petroleum Group Component - Google Patents
A kind of separation system and its separation method of continuous separation petroleum Group Component Download PDFInfo
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- CN109423332A CN109423332A CN201710778480.8A CN201710778480A CN109423332A CN 109423332 A CN109423332 A CN 109423332A CN 201710778480 A CN201710778480 A CN 201710778480A CN 109423332 A CN109423332 A CN 109423332A
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- 238000000926 separation method Methods 0.000 title claims abstract description 138
- 239000003208 petroleum Substances 0.000 title claims abstract description 68
- 239000002904 solvent Substances 0.000 claims abstract description 216
- 238000001179 sorption measurement Methods 0.000 claims abstract description 121
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000001704 evaporation Methods 0.000 claims description 85
- 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 78
- 239000007788 liquid Substances 0.000 claims description 69
- 238000004090 dissolution Methods 0.000 claims description 53
- 238000003795 desorption Methods 0.000 claims description 47
- 239000003205 fragrance Substances 0.000 claims description 42
- 239000000084 colloidal system Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 28
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 19
- 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 16
- 238000000605 extraction Methods 0.000 claims description 14
- 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
- 239000011347 resin Substances 0.000 claims description 11
- 229920005989 resin Polymers 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
- 239000007789 gas Substances 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-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
- 238000010828 elution Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 239000007792 gaseous phase Substances 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000000638 solvent extraction Methods 0.000 claims description 4
- 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
- 238000002156 mixing Methods 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims 1
- 229910002027 silica gel Inorganic materials 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 239000010779 crude oil Substances 0.000 abstract description 17
- 238000004064 recycling Methods 0.000 abstract description 5
- 238000002203 pretreatment Methods 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001944 continuous distillation Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000004821 distillation Methods 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
- 239000011521 glass Substances 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- -1 positive structure Natural products 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000000746 purification 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
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 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
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- C10G53/08—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
-
- 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
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
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)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention discloses the separation system and its separation method of a kind of continuous separation petroleum Group Component.The first adsorption tower top exit and the first evaporator, the rectifying column of the separation system are sequentially connected, and the first adsorption tower outlet at bottom is connected with the material inlet of the second adsorption tower lower part；Second adsorption tower top exit is sequentially connected with the second evaporator, rectifying column；Second adsorption tower outlet at bottom is sequentially connected with third evaporator, extractor, rectifying column；Third evaporator is provided with the entrance of third solvent, and extractor is provided with the entrance of the 4th 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 is connected with the second colvent inlet of the second material entrance of the lower part of the second adsorption tower and top.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 continuous separation petroleum Group Component.
Background technique
Petroleum is mainly made of four kinds of saturation point, fragrance point, resin and asphalt Group Components.Saturation in petroleum, which is divided, includes
Saturated hydrocarbons, such as positive structure, isomery and cycloalkane；Fragrance point includes aromatic hydrocarbon, condensed-nuclei aromatics etc.；Colloid definition is more fuzzy, leads to
Often refer to the dark-coloured colloidal mixture of the higher sulfur-bearing of crude oil middle-molecular-weihydroxyethyl, nitrogen, oxygen；Asphalitine makes the sticky heavy constituent in crude oil,
It is generally difficult to dissolve, be made of the polycyclic compound of high molecular weight.
There are each component respective unique molecule, chemical structure and property, two kinds of crude oil may have completely not in petroleum
With quality and effect, therefore analysis to Group Component in crude oil and calibration are particularly significant.To Various Groups In Crude Oil carry out characterization and
Separation can make refinery, chemical plant etc. that oil property and the market demand be combined to carry out process optimization, in particular for current heavy
Change serious crude oil, guidance can be made for follow-up hydrogenation technological design to the analysis result of Group Component.Such as the glue in crude oil
Hetero atom there are many containing in matter and asphalitine, such as nitrogen, nickel, vanadium, it is subsequent if its fixed composition of a pacing of going forward side by side cannot be isolated
Plus hydrogen, conversion treatment process will have no way of designing or improve, and then influence whole refinery process yields and product quality.
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 is 100~500 times of solvents of conventional separation methods preparation amount.
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.
If CN102527088A discloses a kind of four component separating device of pressure-reducing type asphalt, burnt by glass adsorption column, round bottom
Bottle and depressed control device connect and compose, which is characterized in that the glass adsorption column is equipped with vacuum evacuation device, pumping thereon
Mouth is successively connected with decompressions, flow-dividing control elements such as vacuum meter, protection bottle, vacuum triple valve, four mouthfuls of flow dividers and vacuum pumps；Under
It terminates round-bottomed flask and collects component.Though but it is this analysis, measuring method can semi-automatic four component of measurement content, sample mass
Only 1g further carries out characterizing required gross hereinafter, being unable to satisfy to the structure of organic matter each in asphalitine.
101644698 A of CN provides a kind of chromatogram analysis method of four kinds of Group Components of crude oil, and this method is molten by solvent
Chromatography is solved and carried out, the content of Group Component in crude oil can be measured, however lacks continuous Preparation equipment and separation equipment, nothing
Method handles the crude oil sample of 10g or more and isolated each Group Component.
204188437 U of CN provides in a kind of rock organic solvent separation dress in soluble organic and Various Groups In Crude Oil
It sets.The device can make to evaporate solvent by concatenated water-bath and evaporation panel, and the Group Component under remaining is as product.The party
Method addresses only colloid, the slower problem of solvent evaporation rate in asphalitine purification process, but can not separate different Group Components
When add respectively multi-solvents implement separation；Further, since solvent volatilization process is not provided with circular regeneration equipment, when preparation is big
The safe and environment-friendly problem of solvent volatilization can not ensure when measuring sample.
101070495 B of CN describes a kind of mildization coal-family component separation method based on extraction with back extraction, special
Point is that multiple extraction, back extraction, distillation, washing process are used in series.However this method is suitable for the separation of the coals quality such as raw coal,
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
Miscible with fragrance distribution life, colloid different degrees of can be also dissolved in two kinds of solvents, cause isolated saturation point and fragrance point
Quality forms measurement result substantial deviation reality, 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 crude oil 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 a kind of separation system of continuous separation petroleum Group Component and its divide
From 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, realizes
It operates continuously, the recycling of automatic production and solvent, and after completing a sample separation, next sample can be carried out at once
Separation, do not have to carry out pre-treatment step (washing and replacement adsorption tower etc.).
The present invention provides a kind of separation system of continuous separation petroleum Group Component comprising the first adsorption tower, the second absorption
Tower, the first evaporator, the second evaporator, third evaporator, extractor, rectifying column；
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 is sequentially connected with the first evaporator, rectifying column, the first desorption object outlet of the first absorption tower bottom and the second adsorption tower
The material inlet of lower part is connected；Preferably, the first unadsorbed object outlet and the first evaporator inlet phase at the top of the first adsorption tower
Even, the first evaporation solvent outlet of the first evaporator is connected with rectifying column inlet；
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, rectifying column are sequentially connected, it is preferable that the second unadsorbed object outlet and the second evaporator at the top of the second adsorption tower
Entrance is connected, and the second evaporation solvent outlet of the second evaporator is connected with rectifying column；
Second desorption object outlet of the second absorption tower bottom is sequentially connected with third evaporator, extractor, rectifying column, it is preferable that
Second desorption object outlet of the second absorption tower bottom is connected with the entrance of third evaporator, and the third of third evaporator evaporates outlet
It is connected with extractor entrance, the top taphole of extractor is connected with rectifying column；
Third evaporator is provided with the entrance of third solvent, and extractor is provided with the entrance of the 4th 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 and second
The second material entrance of the lower part of adsorption tower is connected with second colvent inlet on top.
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
The outlet of dissolution unit is connected with the entrance of the second solid-liquid separation unit, and the second mixed dissolution unit preferably includes second
Dissolution kettle, second solid-liquid separation unit preferably include the second drum filter, and second heating unit is used for the
Two dissolution kettles and the second drum filter are heated.
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 steam gaseous phase outlet of first evaporation element is connected with the entrance of rectifying column；
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 steam gaseous phase outlet of second evaporation element is connected with the entrance of rectifying column.
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 includes one of normal heptane, n-hexane, petroleum ether；Second solvent includes one of toluene, benzene；
Third solvent includes 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, macroporous absorption tree is filled in preferably 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.
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, it is further preferred that the side line of rectifying column is provided with the outlet of impurity solvent.
The present invention provides the separation systems and its separation method of a kind of continuous separation petroleum Group Component, use above-mentioned point
The separation of petroleum Group Component is carried out to petroleum from system.
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
Enter the first evaporator with point, then evaporate the first evaporant containing the first solvent, the first evaporant enter rectifying column into
Row rectifying, while saturation point is obtained in the first base of evaporator；
First solvent of rectifying column top exit discharge enters the first adsorption tower from the first colvent inlet, in the first adsorption tower
First adsorbate carries out back flush, desorption, obtains the first desorption object solution, and then the first desorption object solution and the second solvent are mixed
It closes, then again by into the second adsorption tower and occurring from from the material inlet of the first desorption object outlet, the second adsorption tower lower part
Absorption；Unadsorbed the first solvent, the second solvent and fragrance point enters the second evaporator, then evaporates containing the first solvent
With the second evaporant of the second solvent, rectifying is carried out subsequently into rectifying column, while obtaining fragrance point in the second base of evaporator；
Wherein, during or after the first solvent enters the second adsorption tower, the material inlet of the second adsorption tower lower part is also passed through second
Solvent；
Second solvent of rectifier bottoms outlet discharge enters the second adsorption tower from the second colvent inlet, in the second adsorption tower
Second adsorbate carries out back flush, desorption, obtains the second desorption object solution, and then by being exported from the second desorption object,
Third evaporator inlet enters third evaporator, then evaporates the third evaporant containing the second solvent and third solvent, so
Enter extractor afterwards to be extracted, while obtaining colloid in third base of evaporator；Wherein, molten in the second desorption object solution second
During or after agent 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, the 4th solvent
Third solvent is extracted；After the completion of extractor, extractor top contain the extract liquor of the second solvent enter rectifying column into
Row 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 desorption temperature is 50~80 DEG C；The absorption temperature of second adsorption tower
Degree is 20~40 DEG C, and desorption temperature is 50~80 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.
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, progress normal heptane,
The backwash of toluene is desorbed, and there are also the second solvent (toluene), third solvent (ethyl alcohol) is added in proper moment, can be introduced
The not used novel solvent water of conventional separation methods, such technical solution integrally combines, to realize the repetition of adsorption tower
The mixed liquor ability for using, while can also being always ensured that only the first solvent (normal heptane), the second solvent (toluene) or both
Into rectifying column, to realize the first solvent (normal heptane), the separation of the second solvent (toluene) high-purity, reach the mesh of recycling
, and avoid toluene enter saturation point, ethyl alcohol enter saturation point and/or fragrance point, avoid the occurrence of normal heptane-ethyl alcohol-sample,
Normal heptane-miscible the system of toluene-ethano-sample, it is final realize continuous, a large amount of, high-purity, low solvent consumption to crude oil
Sample carries out the purpose of Group component separation, realizes the recycling of continuous operation, automatic production and solvent, and complete one
After sample separation, the separation of next sample can be carried out at once, do not have to carry out pre-treatment step (washing and replacement 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) back flush.
(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 of the embodiment of the present invention 1；
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；A- petroleum；The first solvent of B-；C- second is molten
Agent；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, a kind of separation system of petroleum Group Component of the invention comprising the absorption of the first adsorption tower 3, second
Tower 4, the first evaporator 5, the second evaporator 6, third evaporator 7, extractor 8, rectifying column 9；First adsorption tower 3 is for inhaling
Attached, desorption fragrance point and colloid adsorption tower, the unadsorbed object outlet of the first of 3 top of the first adsorption tower enter with the first evaporator 5
Mouth is connected, and the first desorption object outlet of 3 bottom of the first adsorption tower is connected with the material inlet of 4 lower part of the second adsorption tower；First steams
The first evaporation solvent outlet at 5 top of hair device is connected with rectifying column 9；Second adsorption tower 4 is the absorption for adsorption and desorption colloid
Tower, the unadsorbed object outlet of the second of the top of the second adsorption tower 4 are connected with 6 entrance of the second evaporator, and the of 4 bottom of the second adsorption tower
Two desorption object outlets are connected with the entrance of third evaporator 7；The the second evaporation solvent outlet and 9 phase of rectifying column of second evaporator 6
Even；Third evaporator 7 is provided with the entrance of third solvent, third evaporation outlet and the 8 entrance phase of extractor of third evaporator 7
Even；Extractor 8 is provided with the entrance of the 4th solvent, and the top taphole of extractor 8 is connected with rectifying column 9；The top of rectifying column 9
Portion outlet is connected with the first colvent inlet of top of the first adsorption tower 3；Under the outlet at bottom of rectifying column 9 and the second adsorption tower 4
The second material entrance in portion is connected with second colvent inlet on top.
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 steam gaseous phase outlet of first evaporation element is connected with the entrance of rectifying column 9；Second elutriator
2 are provided with the second evaporation element, and the entrance of second evaporation element is connected with the liquid outlet of the second solid-liquid separation unit, institute
The steam gaseous phase outlet for stating the second evaporation element is connected with the entrance of rectifying column 9.
In another embodiment of the invention, the first evaporator 5 is evaporator for evaporating the first solvent, second
Evaporator 6 is evaporator for evaporate the first solvent and the second solvent, and third evaporator 7 is for the second solvent of evaporation and the
The evaporator of three solvents；Preferably, the evaporation excess of 5 bottom of the first evaporator is exported divides collection device to be connected with saturation, and second
The evaporation excess of 6 bottom of evaporator is exported divides collection device to be connected with fragrance, the evaporation excess of 7 bottom of third evaporator export and
Colloid collection device is connected.It is further preferred that the first evaporator 5, the second evaporator 6 and third evaporator 7 using 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 one of toluene, benzene；The
Three solvents include 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, it is preferable that be filled with macroporous absorption in the first adsorption tower 3
Resin, 5A molecular sieve and alumina packing are filled with macroporous absorbent resin, 5A molecular sieve and silica filler in the second adsorption tower 4.
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.
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 enter the first evaporator 5, then evaporate containing first
The first evaporant of solvent B, the first evaporant enters rectifying column 9 and carries out rectifying, while being saturated in 5 bottom of the first evaporator
Divide F；First solvent B of 9 top exit of rectifying column discharge enters the first adsorption tower 3 from the first colvent inlet, to the first adsorption tower 3
Interior the first adsorbate carries out back flush, desorption, obtains the first desorption object solution, then the first desorption object solution and second molten
Agent mixing, then enter the second adsorption tower 4 from the material inlet of 4 lower part of the second adsorption tower and adsorb；Unadsorbed first
Solvent B, the second solvent C and fragrance point enter the second evaporator 6, then evaporate the containing the first solvent B and the second solvent C
Two evaporants carry out rectifying subsequently into rectifying column 9, while obtaining fragrance in 6 bottom of the second evaporator and dividing G；9 bottom of rectifying column
The second solvent C for exporting discharge enters the second adsorption tower 4 from the second colvent inlet, to the second adsorbate in the second adsorption tower 4
Back flush, desorption are carried out, is obtained containing the second desorption object solution, then enter third evaporator 7 from 7 entrance of third evaporator,
Then the third evaporant containing the second solvent and third solvent is evaporated, is extracted subsequently into extractor 8, while
Three evaporators, 7 bottom obtains colloid H；Wherein, during or after the second desorption object solution enters third evaporator 7, third
7 entrance of evaporator is also passed through third solvent；Before third evaporant enters extraction process, in or after the process, 8 entrance of extractor
It is also passed through the 4th solvent D, the 4th solvent D extracts third solvent；After the completion of extractor 8,8 top of extractor contains second
The rectifying column 9 that enters of the extract liquor of solvent 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 is 1:(0~5), the petroleum being added in the second elutriator 2 is former
Expect, the weight ratio of the second fresh solvent is 1:(0~3).
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, and the first elutriator 1 be added that rectifying column obtains 200 ~
50 ~ 100kg toluene that rectifying column obtains is added in the normal heptane solvent of 500kg, the second elutriator 2.By 0.5kg petroleum A1 and
The mixture of 0.1kg fresh normal heptane is added in the first elutriator 1, then carries out the first mixed dissolution and the first solid-liquid point
From obtaining extracting solution and insoluble matter；The temperature of first mixed dissolution is 85 DEG C, time 5min, the first temperature being separated by solid-liquid separation
It 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, it is dissolved with
Second solvent solution of asphalitine 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 enter
Then first evaporator 5 evaporates normal heptane, and enter rectifying column 9 and carry out rectifying, while obtaining in 5 bottom of the first evaporator
Saturation point, or be further emitted into saturation and divide collection device；The temperature that first evaporator 5 is evaporated is 100~105 DEG C.
After the completion of the absorption of the first adsorption tower 3, the normal heptane of 9 top exit of rectifying column discharge enters from the first colvent inlet
First adsorption tower 3 carries out back flush, desorption to the first adsorbate in the first adsorption tower 3, and desorption temperature is 25 DEG C, is obtained
First desorption object solution, then the first desorption object solution is mixed with toluene, then is discharged from the material inlet of 4 lower part of the second adsorption tower
To the second adsorption tower 4.
(3) first desorption objects enter the second adsorption tower 4(and are filled with macroporous absorbent resin, 5A molecular sieve and silica filler) after
It adsorbs, adsorption temp is 25 DEG C, and unadsorbed normal heptane, toluene and fragrance point enter the second evaporator 6, is then evaporated
The second evaporant containing normal heptane and toluene out carries out rectifying subsequently into rectifying column 9, while in 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 the second adsorption tower 4, the toluene of 9 outlet at bottom of rectifying column discharge enters the from the second colvent inlet
Two adsorption towers 4 carry out back flush, desorption to the second adsorbate in the second adsorption tower 4, and desorption temperature is 60 DEG C, obtains the
Two desorption object solution, then enter 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 second desorption object solution enters third evaporator 7,7 entrance of third evaporator is also passed through ethyl alcohol, third evaporator
7 temperature being evaporated are 105.0~110.6 DEG C；Enter in extraction process in third evaporant, 8 entrance of extractor is also passed through
Water, water extract ethyl alcohol；After the completion of extractor 8,8 top of extractor extract liquor containing toluene enter rectifying column 9 into
Row rectifying.
(5) when all raw materials enter system and after being sufficiently separated, the no longer isolated new product of products export will
The normal heptane of rectifying column, toluene outlet switch to solvent storage device, and the operation of holding system is until all solvents are sufficiently recycled.
Recovered solvent can be used for separation process next time.
Embodiment 2
(2) method of the present embodiment is substantially same as Example 1, difference in: embodiment 1 complete petroleum four components separation
Afterwards, it changes another petroleum A2 and continues the separation of four components.When all raw materials enter system and after being sufficiently separated, produce
Product export no longer isolated new product, and the normal heptane of rectifying column, toluene outlet are switched to solvent storage device, keep system
System operation is until all solvents are sufficiently recycled.Recovered solvent can be used for 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 | 2000 | 200 | 2500 |
| Toluene consumption, g | 200 | 2000 | 200 | 2500 |
| Unit Materials Solvents consumption, g/g | 350 | 11 | 400 | 8 |
| Measurement saturation point, % | 19.31 | 18.90 | 30.21 | 29.89 |
| Measurement fragrance point, % | 47.23 | 47.15 | 55.49 | 53.55 |
| Measure colloid, % | 27.91 | 28.34 | 12.87 | 15.08 |
| Measure asphalitine, % | 5.55 | 5.61 | 1.44 | 1.48 |
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, it can be by appointing
What suitable mode carries out any combination, equally fall into it is disclosed in this invention within the scope of.In addition, it is of the invention it is various not
Any combination can also be carried out between same embodiment, as long as it does not violate the idea of the present invention, equally should be considered as this
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 (21)
1. a kind of separation system of continuous separation petroleum Group Component, which is characterized in that it includes the first adsorption tower, the second absorption
Tower, the first evaporator, the second evaporator, third evaporator, extractor, rectifying column；
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 is sequentially connected with the first evaporator, rectifying column, the first desorption object outlet of the first absorption tower bottom and the second adsorption tower
The material inlet of lower part is connected；
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, rectifying column are sequentially connected；Second absorption tower bottom second desorption object outlet with third evaporator, extractor,
Rectifying column is sequentially connected；Third evaporator is provided with the entrance of third solvent, and extractor is provided with the entrance of the 4th 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 and second
The second material entrance of the lower part of adsorption tower is connected with second colvent inlet on top.
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
The outlet of dissolution unit is connected with the entrance of the second solid-liquid separation unit, and the second mixed dissolution unit preferably includes second
Dissolution kettle, second solid-liquid separation unit preferably include the second drum filter, and second heating unit is used for the
Two dissolution kettles and the second drum filter are heated.
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, the steam gas of first evaporation element
Mutually outlet is connected with the entrance of rectifying column；
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 steam gaseous phase outlet of second evaporation element is connected with the entrance of rectifying column.
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 includes normal heptane, n-hexane, petroleum ether
One of；Second solvent includes one of toluene, benzene；Third solvent includes one of ethyl alcohol, methanol, propyl alcohol；4th
Solvent is 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: 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 is the outlet of high boiling second solvent, it is further preferred that rectifying column
Side line be provided with the outlet of impurity solvent.
12. a kind of separation method of continuous separation petroleum Group Component, it is characterised in that: use separation described in claim 1-11
System carries out the separation of petroleum Group Component to petroleum.
13. separation method as claimed in claim 12, 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
Enter the first evaporator with point, then evaporate the first evaporant containing the first solvent, the first evaporant enter rectifying column into
Row rectifying, while saturation point is obtained in the first base of evaporator；
First solvent of rectifying column top exit discharge enters the first adsorption tower from the first colvent inlet, in the first adsorption tower
First adsorbate carries out back flush, desorption, obtains the first desorption object solution, and then the first desorption object solution and the second solvent are mixed
It closes, then enters the second adsorption tower from the material inlet of the second adsorption tower lower part and adsorb；Unadsorbed the first solvent,
Two solvents and fragrance point enter the second evaporator, then evaporate the second evaporant containing the first solvent and the second solvent, so
Enter rectifying column afterwards and carry out rectifying, while obtaining fragrance point in the second base of evaporator；
Second solvent of rectifier bottoms outlet discharge enters the second adsorption tower from the second colvent inlet, in the second adsorption tower
Second adsorbate carries out back flush, desorption, obtains the second desorption object solution, then enters third from third evaporator inlet and steams
Device is sent out, the third evaporant containing the second solvent and third solvent is then evaporated, is extracted subsequently into extractor, simultaneously
Colloid is obtained in third base of evaporator；Wherein, during or after the second desorption object solution 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, the 4th solvent
Third solvent is extracted；After the completion of extractor, extractor top contain the extract liquor of the second solvent enter rectifying column into
Row rectifying.
14. separation method as claimed in claim 13, 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.
15. separation method as claimed in claim 14, 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.
16. separation method as claimed in claim 13, 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).
17. separation method as claimed in claim 13, it is characterised in that: the adsorption temp of the first adsorption tower is 20~40 DEG C,
Desorption temperature is 50~80 DEG C；The adsorption temp of second adsorption tower is 20~40 DEG C, and desorption temperature is 50~80 DEG C.
18. separation method as claimed in claim 13, 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, and the temperature that third evaporator is evaporated is
105.0~110.6 DEG C.
19. separation method as claimed in claim 13, it is characterised in that: the weight of petroleum and third solvent, the 4th solvent
Amount ratio is 1:(0~2): (10~100).
20. separation method as claimed in claim 13, 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.
21. separation method as claimed in claim 13, 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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Effective date of registration: 20230825 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. |