CN109134182B - Separation system and separation process for product gas and catalyst in reaction of preparing olefin from methanol - Google Patents
Separation system and separation process for product gas and catalyst in reaction of preparing olefin from methanol Download PDFInfo
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- CN109134182B CN109134182B CN201810953605.0A CN201810953605A CN109134182B CN 109134182 B CN109134182 B CN 109134182B CN 201810953605 A CN201810953605 A CN 201810953605A CN 109134182 B CN109134182 B CN 109134182B
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000003054 catalyst Substances 0.000 title claims abstract description 119
- 238000000926 separation method Methods 0.000 title claims abstract description 66
- 150000001336 alkenes Chemical class 0.000 title claims abstract description 50
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 96
- 239000000843 powder Substances 0.000 claims abstract description 46
- 239000012495 reaction gas Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 26
- 239000007795 chemical reaction product Substances 0.000 claims description 59
- 239000000428 dust Substances 0.000 claims description 27
- 239000012528 membrane Substances 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 238000010791 quenching Methods 0.000 abstract description 11
- 230000000171 quenching effect Effects 0.000 abstract description 11
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000003911 water pollution Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 239000007787 solid Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- IAQRGUVFOMOMEM-ARJAWSKDSA-N cis-but-2-ene Chemical compound C\C=C/C IAQRGUVFOMOMEM-ARJAWSKDSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- IAQRGUVFOMOMEM-ONEGZZNKSA-N trans-but-2-ene Chemical compound C\C=C\C IAQRGUVFOMOMEM-ONEGZZNKSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/40—Ethylene production
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a separation system and a separation process of a product gas and a catalyst in a reaction for preparing olefin from methanol, wherein a high-temperature catalyst removal device and an oxide washing tower are arranged at the downstream of a methanol-reaction gas heat exchanger, a three-stage cyclone separator of the original reaction gas is eliminated, so that the catalyst fine powder removal process is simple and efficient, secondary water pollution generated by a quenching tower is eliminated, the process index requirements of the separation of the olefin from the methanol are met, and the system operation period is prolonged.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and relates to a catalyst fine powder removal process carried in reaction product gas of an industrial device for preparing olefin from methanol.
Background
Ethylene and propylene are important basic raw materials in the chemical industry. Conventional olefin production routes require the consumption of large amounts of petroleum. With the rapid increase of the demand for olefins in the chemical industry, the contradiction between supply and demand is increasingly prominent. Therefore, a new process for producing ethylene and propylene by using coal and natural gas as raw materials is developed. The key technology of this new process is the Methanol To Olefins (MTO) technology, which mostly employs a reaction regeneration system in the form of a fluidized bed, and the problem that is common to fluidized beds is that catalyst fines are entrained in the reaction product gas, which must be removed before entering the olefin separation unit. Although the reaction regeneration system is designed with a rapid cyclone separation facility, the separation effect of the product gas and the catalyst fine powder cannot meet the inlet requirement of a compressor of an olefin separation unit under the influence of the limitations of equipment, and therefore the reaction product gas still needs to be washed to realize the fine separation of the reaction product gas and the catalyst fine powder, and the risk of secondary pollution is increased. In the reaction process of preparing olefin (MTO) from methanol according to the reaction mechanism, 56.25% of methanol raw materials are converted into water, a set of 180 ten thousand tons/year methanol-to-olefin device can generate about 116 ten thousand tons/year process water, the process water can be condensed in the water washing process, and the existence of catalyst fine powder can cause great process wastewater treatment pressure.
In order to remove catalyst fine powder carried in reaction product gas, a quenching tower is arranged between a methanol-reaction gas heat exchanger and a water washing tower, and the product gas is cooled and washed by adopting a water washing process, so that the defects are that secondary pollution is generated and water consumption and energy consumption are increased. Chinese patent CN103214333a discloses "an olefin product gas-solid separation and heat exchange system of organic oxygenates": on the basis of analysis of separation effect of a three-stage cyclone separator, the system adopts a technical scheme that a filter is introduced between the upstream of the quenching tower and the downstream of the three-stage cyclone separator (reducing the temperature of MTO products from 480 ℃ to 270-340 ℃) aiming at the damage caused by enrichment of unremoved catalyst fine powder in a subsequent MTO product heat exchanger, a quenching tower, a water scrubber, an olefin separation tower bottom reboiler, a quenching water air cooler, a propylene rectifying tower bottom reboiler, a water scrubber dry air cooler and the like. The disadvantages or problems faced by the separation process of this system are: the three-stage cyclone separator of the reactor has poor separation effect. The design purpose of the three-stage cyclone separator of the reactor is to recover the catalyst lost from the reactor in the start-up and shutdown stage, and the actual operation condition of the device is inspected to find that the catalyst fine powder recovered from the three-stage cyclone separator of the reactor is not much and the gas-solid separation effect is poor.
In addition, the pressure drop of the reaction gas passing through the three-stage cyclone separator is over 200Pa, and catalyst fine powder which is less than 10 mu m and carried by the reaction gas in the methanol-reaction gas heat exchanger can be deposited due to the increase of the pressure drop, so that the inner wall of the methanol-reaction gas heat exchanger is scaled, and the heat exchange efficiency and the system separation efficiency are reduced. And professional equipment and a cleaning agent (Ca (OH) 2) are required for cleaning scale, so that exogenous chemical pollution is easy to introduce, the operation period of the system is shortened, and therefore, the optimization of a product gas and catalyst separation system is needed.
Disclosure of Invention
The invention aims to provide a separation system and a separation process of a product gas and a catalyst in a reaction for preparing olefin from methanol, which not only improve the removal efficiency of catalyst fine powder in the product gas in the reaction for preparing olefin from methanol, but also optimize the process flow, meet the technological index requirements of separation of the product gas and the catalyst in the reaction for preparing olefin from methanol, and improve the operation period of the system.
In order to achieve the above purpose, the invention adopts the following technical scheme:
The utility model provides a reaction product gas and catalyst separation system of methyl alcohol system olefin, including methyl alcohol-reaction gas heat exchanger, high temperature catalyst desorption equipment and oxide scrubbing tower, the reaction product gas outlet of methyl alcohol-reaction gas heat exchanger is linked together with the air inlet side of the built-in dust removal filter core of high temperature catalyst desorption equipment, and the methyl alcohol outlet of methyl alcohol-reaction gas heat exchanger links to each other with the methyl alcohol import of methyl alcohol system olefin reactor, and the reaction product gas inlet of methyl alcohol-reaction gas heat exchanger links to each other with the two-stage cyclone that sets up in the reaction product gas outlet of methyl alcohol system olefin reactor, the air-out side of dust removal filter core links to each other with the gas inlet of oxide scrubbing tower, and the gas outlet of oxide scrubbing tower links to each other with olefin separation unit.
Preferably, the high temperature catalyst removing devices are arranged in two groups (each group comprises 1 or more high temperature catalyst removing devices connected in parallel), and the two groups of high temperature catalyst removing devices are arranged one by one.
Preferably, the high temperature catalyst removing device is provided with a catalyst fine powder collecting assembly, the assembly comprises a differential pressure sensor for collecting pressure difference of inlet and outlet air sides of the filter element, a filter element blowback pipeline communicated with the outlet air side of the filter element and a catalyst fine powder collecting pipeline communicated with the inlet air side of the filter element, the filter element blowback pipeline is connected with a C4 gas source at the top of the debutanizer tower of the olefin separating unit, and the catalyst fine powder collecting pipeline is connected with an external storage tank, so that pressure difference alarm can be utilized, and filter element blowback achieves the purposes of catalyst fine powder removal (filter element regeneration) and catalyst fine powder collection.
Preferably, the dust-removing filter element adopts a high-temperature membrane element, wherein the aperture of a membrane layer of the high-temperature membrane element is 0.5-5 mu m, the aperture of a supporting layer is 30-50 mu m, the membrane layer is mullite particles, the supporting layer is made of silicon carbide material, the flexural strength is more than 20MPa, the porosity is about 37%, the highest temperature resistance is 800 ℃, and the length of the high-temperature membrane element is 0.3-3m (the high-temperature membrane element is customized by manufacturers according to the technical parameters and requirements).
Preferably, the dust interception particle size of the dust removing filter element is less than or equal to 0.3 mu m, and the dust content of the gas filtered by the filter element is less than or equal to 5mg/m 3.
Preferably, the oxide washing tower adopts a gas-liquid parallel flow jet plate tower, and the washing medium is water.
A separation process of a reaction product gas and a catalyst for preparing olefin from methanol comprises the following steps:
And (3) primarily separating catalyst fine powder carried by the reaction product gas from the reaction product gas output by the reactor for preparing olefin from methanol by a two-stage cyclone separator, exchanging heat with saturated methanol steam in a methanol-reaction gas heat exchanger, enabling the reaction product gas cooled by the methanol-reaction gas heat exchanger to enter high-temperature catalyst removal equipment, continuously separating the catalyst fine powder carried by the reaction product gas by a dust removal filter element, cooling and recycling oxygen-containing compounds by an oxide washing tower, and then enabling the reaction product gas to enter an olefin separation unit.
Preferably, the reaction product gas output from the methanol-to-olefin reactor is subjected to two-stage gas-solid separation (primary separation of catalyst fine powder) through a primary cyclone separator and a secondary cyclone separator which are arranged in the methanol-to-olefin reactor, a three-stage cyclone separator is not arranged at the outlet of the reactor, after the two-stage gas-solid separation, the content of the catalyst fine powder in the reaction product gas is 350-450mg/Nm 3, and the particle size distribution (typical value) is 0-10 mu m:87.37%, 10-20 μm:8.78%, 20-40 μm:1.51 percent of the catalyst directly enters a methanol-reaction gas heat exchanger to exchange heat with saturated methanol steam.
Preferably, after heat exchange by a methanol-reaction gas heat exchanger, the temperature of the reaction product gas is reduced from 478-480 ℃ to 260-280 ℃, the temperature of saturated methanol steam is increased from 95-107 ℃ to 200-255 ℃ to form superheated methanol steam, the cooled reaction product gas enters high-temperature catalyst removal equipment, and is filtered by a dust removal filter element to output clean reaction product gas, wherein the content of catalyst fine powder in the reaction product gas is less than or equal to 5mg/m 3, and the particle size distribution (typical value) of the catalyst fine powder is 0.1-0.5 mu m:98.93%, 0.5-5 μm:1.07 percent, the superheated methanol steam enters a reactor for preparing olefin from methanol to react with a catalyst.
Preferably, the operation of the high temperature catalyst removal device comprises three processes of filtering, back blowing and ash discharging, when detecting that the pressure difference of the inlet side and the outlet side of a dust removal filter element in the high temperature catalyst removal device running the filtering process currently is larger than a set value, the filtering process is switched to the standby high temperature catalyst removal device to continue to run, the filter element is back blown, the back blowing medium is C4 gas from the top of the debutanizer tower of the olefin separation unit, separated catalyst fine powder is collected into a storage tank through ash discharging, and the high temperature catalyst removal device corresponding to the filter element can be used as the standby high temperature catalyst removal device after back blowing and ash discharging.
Preferably, the oxide washing tower is mainly used for reducing the temperature of the reaction product gas to 38-44 ℃ and recovering water, dimethyl ether, unreacted methanol and other oxygen-containing compounds generated in the reaction process, and reaching the conditions (typical values) required by the feeding of an olefin separation unit: the temperature is 40 ℃ and the pressure is 0.056MPa (g).
The beneficial effects of the invention are as follows:
The invention sequentially sets high-temperature catalyst removing equipment and an oxide washing tower at the downstream of the methanol-reaction gas heat exchanger, so that the separation of catalyst fine powder in the reaction product gas is changed from liquid-solid separation into gas-solid separation, the three-stage cyclone separator and the quenching tower of the original reaction gas are eliminated, the catalyst fine powder removing process is simpler and more efficient, the separation system can stably run for a long time, the secondary water pollution generated by the quenching tower is eliminated, the process index requirements of the separation of methanol to olefin and olefin are met, and the separated reaction product gas can be directly subjected to olefin separation to obtain a polymerization grade ethylene/propylene product.
Furthermore, the high-temperature catalyst removing equipment is arranged, the separation of the reaction product gas and the catalyst fine powder is realized by utilizing the gas-solid separation principle, and the high-temperature catalyst removing equipment adopts a high-temperature membrane element as a filter element, so that the catalyst fine powder is separated by surface filtration, the porosity is high, the filtration flux is large, the separation effect is stable, the filtration precision is high, the secondary pollution caused by the fact that the catalyst fine powder enters an oxide washing tower is avoided, the process requirement is met, and the difficulty of removing the catalyst solid from the process water is avoided.
Drawings
FIG. 1 is a schematic diagram of a separation system according to the present invention;
In the figure: 1 is a reactor, 2 is a methanol-reaction gas heat exchanger, 3 is catalyst removal equipment, 4 is an oxide washing tower, and 5 is a filter element; PDI: a differential pressure sensor; a: superheated methanol gas is fed into a reactor pipeline; b: a reaction product gas to methanol-reaction gas heat exchanger line; c: a reaction product gas to high temperature catalyst removal equipment pipeline; d: saturated methanol gas comes from the upstream pipeline; e: blowback line (blowback medium from the debutanizer overhead C4 gas from the olefin separation unit); f: the reaction product gas from which the catalyst is removed enters an oxide washing tower pipeline; g: a catalyst fines to spent catalyst storage tank line; h: a reaction product gas to olefin separation unit line; i: wash water to oxide recovery unit line.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
The invention optimizes the system process according to the characteristics of the reaction product gas in the industrial device for preparing olefin from methanol, and in the optimized treatment process, the reaction product gas enters high-temperature catalyst removal equipment after being cooled by a methanol-reaction gas heat exchanger, enters an oxide washing tower after catalyst fine powder is removed, and enters an olefin separation unit after further cooling and oxygen-containing compound recovery.
Referring to fig. 1, the combined process for separating the product gas from the catalyst in the reaction for preparing the olefin by using the methanol provided by the invention comprises a reactor 1 for preparing the olefin by using the methanol, a methanol-reaction gas heat exchanger 2, a high-temperature catalyst removing device 3, an oxide washing tower 4 and a filter element 5 (adopting a high-temperature membrane element).
The reactor 1 for preparing olefin from methanol adopts a turbulent bed reactor (comprising a dense-phase region and a dilute-phase region), the reaction temperature is 480+/-5 ℃, the reaction pressure is 0.12MPa, superheated methanol steam enters the reactor through a feed distributor, methane (containing hydrogen), ethane, ethylene, propane, propylene, C4, C5+, coke, water and the like are generated by contact reaction between the dense-phase region and a catalyst, and the reaction product gas still carries part of catalyst fine powder after being treated by a primary cyclone separator and a secondary cyclone separator and is discharged out of the reactor 1 and enters a methanol-reaction gas heat exchanger 2.
The methanol-reaction gas heat exchanger 2 is a floating head heat exchanger, and the saturated methanol steam is heated by the reaction product gas at a high temperature, the temperature of the reaction product gas is reduced from 478 ℃ to 260 ℃, and the feeding temperature of the high-temperature catalyst removal device 3 is reached.
The high-temperature catalyst removing device 3 is a dust remover, the working principle is similar to that of a bag type dust remover, and the traditional bag type dust remover adopts fiber or filter cloth as a filter element, so that the high-temperature catalyst removing device is low in temperature resistance and short in operation period; the device adopts the high-temperature membrane element as the filter element of the dust remover, and has the advantages of high temperature resistance, corrosion resistance, high strength, high gas permeation flux and strong regeneration performance of the filter element. The high-temperature catalyst removing device 3 is provided with two groups (a plurality of groups can be connected in parallel) which are one on each side and one on each other, and the content of the fine powder of the outlet catalyst is less than or equal to 5mg/m 3.
The oxide washing tower 4 is a gas-liquid parallel flow jet plate tower and is used for treating clean reaction product gas from the high-temperature catalyst removal equipment 3, recovering reaction product water and oxygen-containing compounds such as methanol (unreacted methanol) and dimethyl ether in the product gas, and the temperature of the product gas is reduced from 260 ℃ to 38 ℃ and then enters an olefin separation unit for treatment.
The flow of the combined process for separating the product gas from the catalyst in the reaction of preparing the olefin from the methanol is as follows:
(1) The catalyst fine powder carried by the reaction product gas from the reactor 1 is directly subjected to heat exchange with a methanol-reaction gas heat exchanger 2, the saturated methanol steam temperature is increased from 107 ℃ to 255 ℃ and enters the reactor 1 to participate in the reaction, the reaction product gas temperature is reduced from 478 ℃ to 260 ℃ and enters a high-temperature catalyst removal device 3 to carry out gas-solid separation, the clean reaction product gas is cooled by an oxide washing tower 4 and directly enters an olefin separation unit after the oxygen-containing compound is recovered, and the separated catalyst fine powder enters a spent catalyst storage tank through a collecting pipeline.
(2) As the catalyst fines trapped on the surface of the filter element 5 increases, the pressure difference between the front and rear of the filter element 5 increases, and when the pressure difference is greater than a set value, the filter element 5 needs to be back-blown, and the high-temperature catalyst removal device 3 is switched to another set of operation. The back blowing medium of the filter core adopts the C4 gas (the typical composition is as follows, C3 is below 0.01%, C5 is above 0.15%, n-butane is 4.31%, isobutane is 0.09%, 1-butene is 25.21%, isobutene is 3.86%, cis-2-butene is 7.16%, trans-2-butene is 7.61%, 1, 3-butadiene is 1.59%) at the top of the debutanizer tower of the olefin separation unit, the catalyst fine powder which is blown back is collected to the cone at the lower part of the high-temperature catalyst removal device 3, and when the catalyst fine powder reaches a certain material level height, the catalyst fine powder is discharged to a waste catalyst storage tank.
The invention has the main advantages and characteristics as follows:
(1) The invention optimizes the process flow of a separation system, and the outlet of the reactor is directly connected with a methanol-reaction gas heat exchanger. From the practical operation effect, the three-stage cyclone separator of the reactor is omitted, so that the linear speed of the gas entering the methanol-reactant gas heat exchanger is increased, the temperature loss is reduced, the high-linear speed reactant gas forms self-flushing characteristics in the methanol-reactant gas heat exchanger, catalyst fine powder in the reactant gas cannot deposit and scale, the anti-scaling capacity of the methanol-reactant gas heat exchanger is increased, and the system operation period is prolonged.
(2) The product gas outlet of the high-temperature catalyst removal equipment is directly connected with an oxide washing tower. The content of the catalyst fine powder in the reaction product gas at the outlet of the high-temperature catalyst removing device is less than or equal to 5mg/m 3, and the ultra-low emission standard is achieved. Therefore, the trace catalyst fine powder in the washing water after passing through the peroxide washing tower can not influence the operation of the equipment such as the oxide washing tower, the heat exchanger and the like, and can realize long-period operation.
(3) The oxide washing tower provided by the invention adopts a gas-liquid parallel flow jet type plate tower, compared with a floating valve type tower plate, the gas-liquid flow of the gas-liquid parallel flow jet type tower plate is improved by 50-100%, the efficiency of the tower plate is improved by 10%, the pressure drop of the tower plate is reduced by 10-40%, the operation elasticity is improved by 50%, and meanwhile, the anti-blocking capacity of the washing tower is improved. Thus, the oxide scrubber enhances system stability and operational flexibility.
(4) When the high-temperature catalyst removing equipment performs a filtering process (gas-solid separation), the gas containing the catalyst is filtered through the filter element from outside to inside; when the back-flushing flow is carried out, the back-flushing medium regenerates the filter element from inside to outside. The blowback off gas may continue to enter the reactant gas system to minimize the introduction of non-reaction product components (e.g., inert components) into the system when the blowback medium is selected. Therefore, N 2 is not selected as the blowback medium, the N 2 content in methane hydrogen at the top of the olefin separation unit demethanizer is up to 30%, and the addition of N 2 can increase the load of a reaction gas compressor and influence the separation capacity of the high-pressure depropanizer and the demethanizer, so that the whole system is fluctuated. The C4 gas component at the top of the debutanizer of the olefin separation unit does not contain inert components, has small influence on a reaction gas compressor and a separation system, and is selected as a blowback medium.
(5) The invention not only reduces the quenching tower, but also omits the equipment such as a quenching tower bottom pump, a quenching water cyclone liquid separator, a quenching water filter and the like, optimizes the process flow, reduces the equipment investment and enhances the environmental benefit.
Claims (5)
1. A reaction product gas and catalyst separation system for preparing olefin from methanol is characterized in that: the device comprises a methanol-reaction gas heat exchanger (2), a catalyst removal device (3) and an oxide washing tower (4), wherein a reaction product gas outlet of the methanol-reaction gas heat exchanger (2) is communicated with an air inlet side of a dust removal filter element (5) arranged in the catalyst removal device (3), a methanol outlet of the methanol-reaction gas heat exchanger (2) is connected with a methanol inlet of a methanol-to-olefin reactor (1), a reaction product gas inlet of the methanol-reaction gas heat exchanger (2) is connected with a two-stage cyclone separator arranged at the reaction product gas outlet of the methanol-to-olefin reactor (1), an air outlet side of the dust removal filter element (5) is connected with a gas inlet of the oxide washing tower (4), and a gas outlet of the oxide washing tower (4) is connected with an olefin separation unit;
The catalyst removal equipment (3) is provided with a catalyst fine powder collection assembly which comprises a differential pressure sensor for collecting pressure difference between an inlet pressure and an outlet pressure of the dust removal filter element (5), a filter element blowback pipeline communicated with the outlet side of the dust removal filter element (5) and a catalyst fine powder collection pipeline communicated with the inlet side of the dust removal filter element (5), wherein the filter element blowback pipeline is connected with a C4 gas source at the top of the debutanizer of the olefin separation unit, and the catalyst fine powder collection pipeline is connected with an external storage tank;
The dust-removing filter element (5) adopts a high-temperature membrane element, the aperture of a membrane layer of the high-temperature membrane element is 0.5-5 mu m, the aperture of a supporting layer is 30-50 mu m, the membrane layer is mullite particles, the supporting layer is made of silicon carbide material, the flexural strength is more than 20MPa, and the maximum temperature resistance is 800 ℃, and the length is 0.3-3m;
The dust interception particle size of the dust removing filter element (5) is less than or equal to 0.3 mu m, and the dust content of the gas filtered by the dust removing filter element (5) is less than or equal to 5mg/m 3.
2. The methanol-to-olefins reaction product gas and catalyst separation system of claim 1, wherein: the catalyst removing devices (3) are arranged in two groups, and the two groups of catalyst removing devices (3) are one on one side and one on the other side.
3. The methanol-to-olefins reaction product gas and catalyst separation system of claim 1, wherein: the oxide washing tower (4) adopts a gas-liquid parallel flow jet plate tower.
4. A separation process of a reaction product gas and a catalyst for preparing olefin from methanol is characterized by comprising the following steps: the method comprises the following steps: the method comprises the steps that reaction product gas output from a reactor (1) for preparing olefin from methanol is subjected to primary separation of catalyst fine powder carried by the reaction product gas through a two-stage cyclone separator, then is subjected to heat exchange with saturated methanol steam in a methanol-reaction gas heat exchanger (2), the reaction product gas cooled through the methanol-reaction gas heat exchanger (2) enters a catalyst removal device (3), catalyst fine powder carried by the reaction product gas is continuously separated through a dust removal filter element (5) arranged in the catalyst removal device (3), and clean reaction product gas obtained through separation is subjected to cooling through an oxide washing tower (4) and is subjected to recovery of oxygen-containing compounds and then enters an olefin separation unit;
The dust-removing filter element (5) adopts a high-temperature membrane element, the aperture of a membrane layer of the high-temperature membrane element is 0.5-5 mu m, the aperture of a supporting layer is 30-50 mu m, the membrane layer is mullite particles, the supporting layer is made of silicon carbide material, the flexural strength is more than 20MPa, and the maximum temperature resistance is 800 ℃, and the length is 0.3-3m;
After heat exchange by a methanol-reaction gas heat exchanger (2), the temperature of the reaction product gas is reduced from 478-480 ℃ to 260-280 ℃, the temperature of saturated methanol steam is increased from 95-107 ℃ to 200-255 ℃ to form superheated methanol steam, the cooled reaction product gas enters a catalyst removal device (3), and the cooled reaction product gas is filtered by a dust removal filter element (5) to output clean reaction product gas, wherein the content of catalyst fine powder in the reaction product gas is less than or equal to 5mg/m 3, and the superheated methanol steam enters a methanol-to-olefin reactor (1);
The operation of the catalyst removal device (3) comprises three processes of filtering, back blowing and ash discharging, when detecting that the pressure difference of the inlet side and the outlet side of a dust removal filter element (5) in the catalyst removal device (3) of the current operation filtering process is larger than a set value, the filtering process is switched to the standby catalyst removal device (3) to continue to operate, then the back blowing is carried out on the dust removal filter element (5), the back blowing medium is C4 gas from the top of a debutanizer tower of an olefin separation unit, catalyst fine powder separated from the dust removal filter element (5) is collected into an external storage tank through ash discharging, and the catalyst removal device (3) corresponding to the dust removal filter element (5) is used as the standby catalyst removal device (3) after the back blowing and the ash discharging.
5. The process for separating product gas from catalyst in a methanol-to-olefins reaction according to claim 4, wherein: after separation by a two-stage cyclone separator, the content of the catalyst fine powder in the reaction product gas is 350-450mg/m 3.
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| US20200298224A1 (en) * | 2019-03-21 | 2020-09-24 | Kellogg Brown & Root Llc | System and method for catalyst removal from mto effluent |
| CN113620765B (en) * | 2020-05-08 | 2023-09-08 | 中石化洛阳工程有限公司 | Pretreatment method and equipment for reaction generated gas in process of preparing olefin from oxygen-containing compound |
| CN112179872A (en) * | 2020-10-22 | 2021-01-05 | 陕西延长中煤榆林能源化工有限公司 | Method for rapidly determining moisture content in MTO-grade methanol by using refraction method |
| CN115253921B (en) * | 2022-05-25 | 2024-12-10 | 中国神华煤制油化工有限公司 | A circulation system for protecting high-temperature pipelines by quenching and solidification |
| CN116786037A (en) * | 2023-06-27 | 2023-09-22 | 上海润和盛建工程科技有限公司 | System for preparing olefin from methanol |
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