CN109851464B - Method and device for isomerizing n-butene - Google Patents
Method and device for isomerizing n-butene Download PDFInfo
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- CN109851464B CN109851464B CN201711234499.2A CN201711234499A CN109851464B CN 109851464 B CN109851464 B CN 109851464B CN 201711234499 A CN201711234499 A CN 201711234499A CN 109851464 B CN109851464 B CN 109851464B
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- 238000000034 method Methods 0.000 title claims abstract description 43
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 305
- 239000002994 raw material Substances 0.000 claims abstract description 270
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims description 75
- 238000006317 isomerization reaction Methods 0.000 claims description 36
- 239000002808 molecular sieve Substances 0.000 claims description 8
- 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 8
- 230000001172 regenerating effect Effects 0.000 claims description 7
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- 208000012839 conversion disease Diseases 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 abstract description 22
- 239000000047 product Substances 0.000 description 62
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 8
- 150000001336 alkenes Chemical class 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 238000006266 etherification reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- NUMQCACRALPSHD-UHFFFAOYSA-N tert-butyl ethyl ether Chemical compound CCOC(C)(C)C NUMQCACRALPSHD-UHFFFAOYSA-N 0.000 description 4
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003254 gasoline additive Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for isomerizing n-butene, which comprises the following steps: the first raw material is sent to a first reaction zone for reaction; when the temperature of the first reaction zone is raised to 335-; the first raw material exchanges heat with the product flow in the second reaction zone, and then is heated to 335-; when the temperature of the first reaction zone is increased to 355-365 ℃, stopping the reaction in the first reaction zone; when the temperature of the second reaction zone is raised to 335-; the second raw material exchanges heat with the product flow in the first reaction zone, and then is heated to 335-; when the temperature of the second reaction zone is increased to 355-365 ℃, the reaction in the second reaction zone is stopped, and the steps are repeated. By adopting the method and the device, the yield of the isobutene can be increased by 70-80% and the utilization rate of the catalyst and equipment can be increased by 70-80% on the premise of ensuring the product quality.
Description
Technical Field
The invention relates to a method and a device for isomerizing n-butene, in particular to a method for improving the yield of isobutene and improving the utilization rate of a catalyst and equipment by adjusting the connection relation and a process route of a reaction device.
Background
Methyl tert-butyl ether (MTBE) and ethyl tert-butyl ether (ETBE) have the advantages of higher octane number, low vapor pressure and good solubility in gasoline hydrocarbon fractions, so that the MTBE becomes an excellent gasoline additive component and the demand is rapidly increased all over the world. Thus, the isobutene yields obtained by conventional catalytic cracking and thermal processing of petroleum alone have far failed to meet the needs of the production of etherification units. After methanol and ether are separated from the outlet material of the MTBE etherification device, the normal olefin accounts for 40-100 wt%, and if the material rich in n-butene is subjected to skeletal isomerization to produce isobutene, the aim of increasing the yield of isobutene can be achieved; the process has the advantages of low price and easy obtainment of raw materials, sufficient sources and the like, can better solve the problem of surplus linear chain olefin, can provide a large amount of raw materials for an etherification synthesis device, and only needs to add an olefin isomerization device at the downstream of the existing etherification device, thereby becoming the method for increasing the yield of the isoolefins with the most development potential at present.
Molecular sieves are the most commonly used catalysts in n-butene isomerization reactions, with ZSM-35 and SAPO-11 being the most widely used. ZSM-35 zeolite is a molecular sieve with the FER topology developed successfully by Mobil in the late seventies of the United states (U.S. Pat. No. 4,016,245) containing ten-membered ring channels (0.42X 0.54nm) and intersecting eight-membered ring channels (0.35X 0.48 nm). The cross sections of the two pore channels are elliptical, and the pore channels are vertically crossed. The oval pore channels of the ZSM-35 molecular sieve are large enough to allow linear olefins to enter and diffuse isoolefins with methyl branches, and small enough to limit the generation of C3 and C5 bimolecular reaction intermediate C8 byproducts and coking, so that the ZSM-35 molecular sieve is the zeolite catalyst which is discovered to be the best in stability so far, and is very suitable for being applied to the isomerization reaction of normal butene.
The n-butene isomerization reaction is characterized in that the activity of the catalyst at the initial stage is higher, the higher n-butene conversion rate can be achieved at lower reaction temperature, but the isobutene selectivity is low, and the generation amount of C8 byproducts is large; after the catalyst activity is reduced in the middle and later periods of the once-through regeneration period, the reaction temperature needs to be increased to keep the conversion rate of n-butene, the selectivity of isobutene is improved, and the generation amount of byproducts is reduced. When the activity of the catalyst is reduced to the required value, the reaction temperature is increased, and the catalyst is regenerated and continues to operate in the next period.
The ISOMPLUS technology from Lyondell corporation is the most representative process for the isomerization of n-butenes, and a brief process flow is shown in FIG. 1. The n-butene raw material exchanges heat with the material at the outlet of the reactor, enters a heating furnace to be heated to the reaction temperature, enters the reactor to carry out isomerization reaction, and enters a de-weighting tower to separate out heavy components of by-products after the product exchanges heat with the raw material and is pressurized, so that the product rich in isobutene is obtained. In order to realize continuous production of the device, two reactors, two heat exchangers and a heating furnace are generally provided, when one reactor is operated until the catalyst needs to be regenerated, the other reactor is switched, namely, the two reactors are opened and prepared.
From the above description, it can be seen that in the current n-butene isomerization process, only one reactor is usually operated, the utilization rate of the catalyst and the reaction equipment is only 50%, and the capacity of the device is not fully developed.
Disclosure of Invention
The invention aims to provide a method and a device for isomerizing n-butene, aiming at the technical problems in the prior art, and the method and the device can realize that 2 reactors can simultaneously operate within more than 70% of time by designing a novel reaction device for isomerizing n-butene and adjusting the process route of the device, thereby greatly improving the use efficiency of a catalyst and equipment and simultaneously increasing the yield of isobutene.
According to one aspect of the present invention, there is provided a method for isomerizing n-butene, comprising:
s1, sending the first raw material to a first reaction area for reaction, wherein the initial reaction temperature in the first reaction area is 290-300 ℃;
s2, when the isomerization reaction conversion rate in the first reaction zone is lower than 40%, starting to increase the reaction temperature of the first reaction zone;
s3, when the reaction temperature in the first reaction zone is increased to 335-; meanwhile, the first raw material and the product flow of the second reaction zone exchange heat, and then are heated to 335-;
s4, when the reaction temperature in the first reaction zone rises to 355-365 ℃, stopping the reaction in the first reaction zone, regenerating the catalyst in the first reaction zone, and sending the second raw material to the second reaction zone for reaction;
s5, when the isomerization reaction conversion rate in the second reaction zone is lower than 40%, increasing the reaction temperature in the second reaction zone;
s6, when the reaction temperature in the second reaction zone is increased to 335-; meanwhile, the second raw material exchanges heat with the product flow in the first reaction zone, and then is heated to 335-;
s7, when the reaction temperature in the second reaction area rises to 355-365 ℃, stopping the reaction in the second reaction area, regenerating the catalyst in the second reaction area, and sending the first raw material to the first reaction area for reaction;
s8 repeats steps S2-S7.
According to some embodiments of the present invention, in step S1, the first raw material is first heat exchanged with the product stream of the first reaction zone, and then heated by the heating furnace to the reaction temperature of the first reaction zone, and sent to the first reaction zone for reaction.
According to a preferred embodiment of the present invention, during the reaction, when the isomerization conversion in the first reaction zone is less than 40%, the reaction temperature in the first reaction zone is increased by increasing the temperature of the furnace, preferably to maintain the isomerization conversion greater than 40%.
According to some embodiments of the invention, the temperature increase rate in step S2 is 1-3 ℃/day.
According to some embodiments of the present invention, when the temperature in the first reaction zone is 335-345 ℃, the temperature of the product stream is 365-375 ℃; at the moment, the second raw material exchanges heat with the product flow of the second reaction area and the first reaction area in turn, is heated to the temperature of 290-; at the moment, the feeding path and mode of the first raw material are changed, the first raw material exchanges heat with the product flow of the second reaction zone, and then the product flow is heated to 335-.
According to a preferred embodiment of the present invention, in step S3, the feeding amount of the second raw material is determined based on the reaction temperature in the second reaction zone, and the reaction temperature in the second reaction zone is ensured to be not lower than 290 ℃.
According to a preferred embodiment of the present invention, in the step S3, the feeding amount of the second raw material is 60 to 80% of the feeding amount of the first raw material.
According to some embodiments of the present invention, in step S4, the second raw material is first heat exchanged with the product stream of the second reaction zone, and then heated by the heating furnace to the reaction temperature of the second reaction zone, and sent to the second reaction zone for reaction.
According to a preferred embodiment of the present invention, during the reaction, when the isomerization conversion in the second reaction zone is less than 40%, the reaction temperature in the second reaction zone is increased by increasing the temperature of the furnace, preferably to maintain the isomerization conversion greater than 40%.
According to some embodiments of the invention, the temperature increase rate in step S5 is 1-3 ℃/day.
According to some embodiments of the present invention, when the temperature in the second reaction zone is increased to 335-345 ℃, the temperature of the product stream is 365-375 ℃; at the moment, the first raw material exchanges heat with the product flow of the first reaction area and the second reaction area in sequence, is heated to the temperature of 290-; at the moment, the feeding path and mode of the second raw material are changed, the second raw material exchanges heat with the product flow in the first reaction zone, and then is heated to 335-.
According to a preferred embodiment of the present invention, in step S6, the feeding amount of the first raw material is determined according to the reaction temperature in the first reaction zone, so as to ensure that the reaction temperature in the first reaction zone is not lower than 290 ℃; in some specific embodiments, the feed amount of the first raw material is 60 to 80% of the feed amount of the second raw material.
According to some embodiments of the invention, the feedstock comprises n-butenes and a catalyst; and/or the catalyst comprises a ZSM-35 molecular sieve, the silica-alumina ratio of the catalyst is 40-60, and the regeneration period is more than 40 days.
In some specific embodiments, the ZSM-35 molecular sieve seed crystal has a diameter of 300-800nm and a thickness of less than 100 nm; the prepared ZSM-35 molecular sieve is small crystal grains, has an FER (magnesium alkali Buddha stone) structure, and has the crystal grain diameter of 200-700 nm and the thickness of less than 100 nm. The initial reaction temperature of the catalyst is 290 ℃, and the one-way regeneration period is 40 days.
According to a preferred embodiment of the present invention, the time from start-up to the temperature increase to 335-345 ℃ in the first reaction zone or the second reaction zone is 13-15 days; and/or the catalyst in the first reaction zone or the second reaction zone is regenerated for a period of 6 to 7 days.
According to another aspect of the present invention, there is provided an apparatus for isomerizing normal butenes, comprising:
the first reaction zone is used for enabling the raw materials to have n-butene isomerization reaction, and comprises at least one reactor, an inlet and an outlet are arranged on the reactor of the first reaction zone, the inlet is respectively connected with the outlet of the heating furnace and the raw material outlet of the second heat exchanger, and the outlet is connected with the product inlet of the first heat exchanger;
the first heat exchanger is used for exchanging heat between the raw material and the product of the first reaction zone reactor, and is provided with a raw material inlet, a raw material outlet, a product inlet and a product outlet, wherein the raw material inlet is respectively connected with the raw material tank and the raw material outlet of the second heat exchanger, the raw material outlet is respectively connected with the inlet of the heating furnace, the raw material inlet of the second heat exchanger and the inlet of the second reaction zone reactor, and the product outlet outputs the product obtained by the first reaction zone reactor;
the second reaction zone is used for enabling the raw materials to have n-butene isomerization reaction in the second reaction zone and comprises at least one reactor, an inlet and an outlet are arranged on the reactor of the second reaction zone, the inlet is respectively connected with the outlet of the heating furnace and the raw material outlet of the first heat exchanger, and the outlet is connected with the product inlet of the second heat exchanger;
the second heat exchanger is used for exchanging heat between the raw material and the product of the second reaction zone reactor, and is provided with a raw material inlet, a raw material outlet, a product inlet and a product outlet, wherein the raw material inlet is respectively connected with the raw material tank and the raw material outlet of the first heat exchanger, the raw material outlet is respectively connected with the inlet of the heating furnace, the raw material inlet of the first heat exchanger and the inlet of the first reaction zone reactor, and the product outlet outputs the product obtained by the second reaction zone reactor;
the heating furnace is used for heating raw materials, an inlet and an outlet are arranged on the heating furnace, the inlet is respectively connected with the raw material outlet of the first heat exchanger and the raw material outlet of the second heat exchanger, and the outlet is respectively connected with the inlet of the first reaction zone reactor and the inlet of the second reaction zone reactor;
and the pipeline is used for connecting the devices and is provided with a valve.
According to a preferred embodiment of the present invention, the initial reaction temperature in the first reaction zone is 290-300 ℃; and/or the initial reaction temperature in the second reaction zone is 290-300 ℃.
According to some embodiments of the present invention, the time from start-up to the temperature increase to 335-345 ℃ in the first reaction zone or the second reaction zone is 13-15 days; and/or the catalyst in the first reaction zone or the second reaction zone is regenerated for a period of 6 to 7 days.
According to some embodiments of the invention, the inlet of the first reaction zone reactor is connected to the outlet of the heating furnace through a pipeline, and a first valve is arranged on the inlet of the first reaction zone reactor; and the inlet of the first reaction zone reactor is connected with the raw material outlet of the second heat exchanger through a pipeline, and a second valve is arranged on the inlet of the first reaction zone reactor. When the first valve is opened and the second valve is closed, the first reaction zone reactor receives the raw materials from the heating furnace; when the first valve is closed and the second valve is opened, the first reaction zone reactor receives the raw material from the second heat exchanger.
According to some embodiments of the invention, the inlet of the second reaction zone reactor is connected to the outlet of the heating furnace through a pipeline, and a third valve is arranged on the inlet of the second reaction zone reactor; and the inlet of the second reaction zone reactor is connected with the raw material outlet of the first heat exchanger through a pipeline, and a fourth valve is arranged on the inlet of the second reaction zone reactor. When the third valve is opened and the fourth valve is closed, the second reaction area reactor receives the raw materials from the heating furnace; the second reaction zone reactor receives feed from the first heat exchanger when the fourth valve is open and the third valve is closed.
According to some embodiments of the invention, the raw material inlet of the first heat exchanger is connected to the raw material tank through a pipeline, and a fifth valve is arranged on the raw material inlet; the raw material inlet of the first heat exchanger is connected with the raw material outlet of the second heat exchanger through a pipeline, and a sixth valve is arranged on the raw material inlet of the first heat exchanger; when the fifth valve is opened and the sixth valve is closed, the first heat exchanger receives raw materials from the raw material tank; when the fifth valve is closed and the sixth valve is opened, the first heat exchanger receives the raw material from the second heat exchanger.
According to some embodiments of the invention, the raw material outlet of the first heat exchanger is connected with the inlet of the heating furnace through a pipeline, and a seventh valve is arranged on the raw material outlet of the first heat exchanger; the raw material outlet of the first heat exchanger is connected with the raw material inlet of the second heat exchanger through a pipeline, and an eighth valve is arranged on the raw material outlet of the first heat exchanger; the raw material outlet of the first heat exchanger is connected with the inlet of the second reaction zone reactor through a pipeline, and a fourth valve is arranged on the raw material outlet of the first heat exchanger; when the seventh valve is opened and the eighth valve and the fourth valve are closed, the raw material output by the first heat exchanger enters the heating furnace; when the eighth valve is opened and the seventh valve and the fourth valve are closed, the raw material output by the first heat exchanger enters the second heat exchanger; when the fourth valve is opened and the seventh and eighth valves are closed, the raw material output by the first heat exchanger enters the second reaction zone reactor.
According to some embodiments of the invention, the raw material inlet of the second heat exchanger is connected to the raw material tank through a pipeline, and a ninth valve is arranged on the raw material inlet; the raw material inlet of the second heat exchanger is connected with the raw material outlet of the first heat exchanger through a pipeline, and an eighth valve is arranged on the raw material inlet of the second heat exchanger; when the ninth valve is opened and the eighth valve is closed, the second heat exchanger receives the raw material from the raw material tank; when the ninth valve is closed and the eighth valve is opened, the second heat exchanger receives the raw material from the first heat exchanger.
According to some embodiments of the invention, the raw material outlet of the second heat exchanger is connected with the inlet of the heating furnace through a pipeline, and a tenth valve is arranged on the raw material outlet of the second heat exchanger; the raw material outlet of the second heat exchanger is connected with the raw material inlet of the first heat exchanger through a pipeline, and a sixth valve is arranged on the raw material outlet of the second heat exchanger; the raw material outlet of the second heat exchanger is connected with the inlet of the first reaction zone reactor through a pipeline, and a second valve is arranged on the raw material outlet of the second heat exchanger; when the tenth valve is opened and the sixth valve and the second valve are closed, the raw material output by the second heat exchanger enters the heating furnace; when the sixth valve is opened and the tenth valve and the second valve are closed, the raw material output by the second heat exchanger enters the first heat exchanger; when the second valve is opened and the sixth valve and the tenth valve are closed, the raw material output by the second heat exchanger enters the first reaction zone reactor.
According to some embodiments of the present invention, the inlet of the heating furnace is connected to the raw material outlet of the first heat exchanger through a pipeline, and a seventh valve is arranged on the inlet of the heating furnace; the inlet of the heating furnace is connected with the raw material outlet of the second heat exchanger through a pipeline, and a tenth valve is arranged on the heating furnace; when the seventh valve is opened and the tenth valve is closed, the heating furnace receives the raw materials from the first heat exchanger; when the seventh valve is closed and the tenth valve is opened, the heating furnace receives the raw material from the second heat exchanger.
According to some embodiments of the present invention, the outlet of the heating furnace is connected to the inlet of the first reaction zone reactor through a pipe, and a first valve is arranged on the outlet of the heating furnace; the outlet of the heating furnace is connected with the inlet of the second reaction zone reactor through a pipeline, and a third valve is arranged on the outlet of the heating furnace.
According to a preferred embodiment of the present invention, a first flowmeter is disposed on a pipeline between the raw material outlet of the first heat exchanger and the raw material inlet of the second heat exchanger, a second flowmeter is disposed on a pipeline between the raw material outlet of the second heat exchanger and the raw material inlet of the first heat exchanger, a third flowmeter is disposed on a pipeline between the raw material outlet of the first heat exchanger and the inlet of the heating furnace, a fourth flowmeter is disposed on a pipeline between the raw material outlet of the second heat exchanger and the inlet of the heating furnace, and the feeding amounts of the raw materials respectively entering the first reaction zone reactor and the second reaction zone reactor are controlled by adjusting the size of the valve.
According to some embodiments of the present invention, the operation of the n-butene isomerization apparatus according to the present invention is as follows:
opening the first valve, the fifth valve and the seventh valve, closing the third valve, the fourth valve, the eighth valve and the ninth valve, exchanging heat between the first raw material and the product of the first reaction zone reactor in the first heat exchanger, then entering the heating furnace through the raw material outlet of the first heat exchanger to be heated to the temperature of 290 ℃ and 300 ℃, and sending the heated raw material to the first reaction zone reactor for reaction; at the moment, the product obtained by the first reaction zone reactor enters a first heat exchanger through a product inlet; beginning to increase the temperature of the first reaction zone reactor when the isomerization conversion of the first reaction zone reactor is less than 40%;
when the temperature in the first reaction zone reactor reaches 335-345 ℃ (the process is about 13-15 days), the temperature of the outlet product is 365-375 ℃; at this time, starting a second reaction zone reactor, wherein the initial reaction temperature in the second reaction zone reactor is 290-300 ℃; opening first, fourth, sixth, ninth and tenth valves, closing second, third, fifth, seventh and eighth valves, enabling the first raw material and the second raw material to enter a second heat exchanger to exchange heat with a product of a second reaction zone reactor, enabling the second raw material to enter the first heat exchanger, enabling the first raw material to enter a heating furnace, controlling the feeding amount of the first raw material to be unchanged through a second flowmeter and a fourth flowmeter, enabling the feeding amount of the second raw material to be 60-80% of that of the first raw material, enabling the raw material to be heated to 290-phase-changing 300 ℃ from room temperature after the heat exchange between the second raw material and an outlet product of the first reaction zone reactor, and enabling the raw material to enter the second reaction zone reactor to react; heating the first raw material to 335-;
when the reaction temperature in the first reaction zone reactor rises to 355-365 ℃, stopping the first reaction zone reactor, and regenerating the catalyst in the first reaction zone reactor (the process is about 6-7 days); at the moment, opening the third, ninth and tenth valves, closing the first, second, fifth and sixth valves, exchanging heat between the second raw material and the product of the second reaction zone reactor in the second heat exchanger, then entering the heating furnace through the raw material outlet of the second heat exchanger to be heated to the reaction temperature of the second reaction zone reactor, and sending the heated raw material to the second reaction zone reactor for reaction; meanwhile, the feeding amount of the second raw material is increased to be the same as the initial feeding amount of the first raw material; when the isomerization conversion in the second reaction zone reactor is less than 40%, beginning to raise the temperature in the first reaction zone reactor;
when the reaction temperature in the second reaction zone reactor is raised to 335-; opening second, third, fifth, seventh and eighth valves, closing first, fourth, sixth, ninth and tenth valves, allowing the first raw material and the second raw material to enter a first heat exchanger to exchange heat with the product in the first reaction zone reactor, allowing the first raw material to enter a second heat exchanger, heating the raw materials from room temperature to 290 ℃ and 300 ℃, and allowing the raw materials to enter the first reaction zone reactor for reaction; the second raw material enters a heating furnace, is heated to 335-; controlling the feeding amount of the second raw material to be constant through the first flow meter and the third flow meter, wherein the feeding amount of the first raw material is 60-80% of that of the second raw material;
when the reaction temperature in the second reaction zone reactor rises to 355-365 ℃, stopping the second reaction zone reactor and regenerating the catalyst therein (about 6-7 days in the process); opening the first valve, the fifth valve and the seventh valve, closing the third valve, the fourth valve, the eighth valve and the ninth valve, starting the first reaction zone reactor, exchanging heat between the first raw material and a product of the first reaction zone reactor in the first heat exchanger, then entering a heating furnace through a raw material outlet of the first heat exchanger, heating to the temperature of 290 ℃ and 300 ℃, and sending the heated raw material to the first reaction zone reactor for reaction; when the isomerization conversion in the first reaction zone reactor is less than 40%, the temperature in the first reaction zone reactor is initially increased and the above operation is repeated.
According to another aspect of the invention, there is provided a use of the above apparatus for isomerizing normal butenes, comprising performing a reaction using the apparatus for isomerizing normal butenes by:
a1 opening the first, fifth and seventh valves, closing the third, fourth, eighth and ninth valves, starting the first reaction zone reactor, exchanging heat of the first raw material in the first heat exchanger, then entering the heating furnace through the raw material outlet of the first heat exchanger to heat to 290-;
a2 when the isomerization conversion rate of the first reaction zone reactor is lower than 40%, the temperature of the first reaction zone reactor is started to be increased;
a3 when the reaction temperature in the first reaction zone reactor rises to 335-; opening the first, fourth, sixth, ninth and tenth valves, closing the second, third, fifth, seventh and eighth valves, allowing the first raw material and the second raw material to enter a second heat exchanger to exchange heat with the product of the second reaction zone reactor, allowing the second raw material to enter the first heat exchanger, allowing the first raw material to enter a heating furnace, allowing the second raw material to exchange heat with the product at the outlet of the first reaction zone reactor, allowing the raw materials to be heated to 300 ℃ from room temperature, and allowing the raw materials to enter the second reaction zone reactor for reaction; heating the first raw material to 335-;
a4 stopping the first reaction zone reactor when the reaction temperature in the first reaction zone reactor rises to 355-365 ℃ to regenerate the catalyst therein; opening the third, ninth and tenth valves, closing the first, second, fifth and sixth valves, exchanging heat between the second raw material and the product of the second reaction zone reactor in the second heat exchanger, then entering the heating furnace through the raw material outlet of the second heat exchanger, heating to the reaction temperature of the second reaction zone reactor, and sending to the second reaction zone reactor for reaction; meanwhile, the feeding amount of the second raw material is increased to be the same as the initial feeding amount of the first raw material;
a5 when the isomerization conversion rate of the second reaction zone reactor is lower than 40%, the temperature of the first reaction zone reactor is started to be increased;
a6 when the reaction temperature in the second reaction zone reactor rises to 335-; opening second, third, fifth, seventh and eighth valves, closing first, fourth, sixth, ninth and tenth valves, allowing the first raw material and the second raw material to enter a first heat exchanger to exchange heat with the product in the first reaction zone reactor, allowing the first raw material to enter a second heat exchanger, heating the raw materials from room temperature to 290 ℃ and 300 ℃, and allowing the raw materials to enter the first reaction zone reactor for reaction; the second raw material enters a heating furnace, is heated to 335-;
a7 when the reaction temperature in the second reaction zone reactor rises to 355-365 ℃, stopping the second reaction zone reactor and regenerating the catalyst therein (about 6-7 days in the process); opening the first valve, the fifth valve and the seventh valve, closing the third valve, the fourth valve, the eighth valve and the ninth valve, starting the first reaction zone reactor, exchanging heat between the first raw material and a product of the first reaction zone reactor in the first heat exchanger, then entering a heating furnace through a raw material outlet of the first heat exchanger, heating to the temperature of 290 ℃ and 300 ℃, and sending the heated raw material to the first reaction zone reactor for reaction;
a8 repeats the operations of steps A2-A7.
According to some embodiments of the present invention, in step a3, the feeding amount of the first raw material is controlled to be constant by the second flow meter and the fourth flow meter, and the feeding amount of the second raw material is controlled to be 60 to 80% of the first raw material.
According to some embodiments of the present invention, in step a6, the feeding amount of the second raw material is controlled to be constant by the first flow meter and the third flow meter, and the feeding amount of the first raw material is 60 to 80% of the second raw material.
The invention provides a method for isomerizing n-butene, which realizes the potential of the existing equipment on the premise of carrying out detailed analysis on a n-butene isomerization reaction process, simultaneously considers that the reaction temperatures required in different stages of a catalyst operation period are different, and improves a n-butene isomerization device. By adopting the method and the device, the yield of the isobutene can be increased by 70-80% and the utilization rate of the catalyst and equipment can be increased by 70-80% on the premise of ensuring the product quality. Meanwhile, the device and the method of the invention can operate two reactors by only one heating furnace, thereby simplifying the device, being simple and convenient to operate and saving resources.
Drawings
FIG. 1 shows a process flow diagram of a prior art ISOMPLUS technique;
FIG. 2 is a block diagram showing a normal butene isomerization unit according to an embodiment of the present invention;
description of reference numerals: 1. a first reactor; 2. a first heat exchanger; 3. a second reactor; 4. a second heat exchanger; 5. heating furnace; 6. a first valve; 7. a second valve; 8. a third valve; 9. a fourth valve; 10. a fifth valve; 11. a sixth valve; 12. a seventh valve; 13. an eighth valve; 14. a ninth valve; 15. a tenth valve; 16. a first flow meter; 17. a second flow meter; 18. a third flow meter; 19. and a fourth flow meter.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
As shown in fig. 2, according to an embodiment of the present invention, the apparatus for isomerizing normal butenes of the present invention comprises a first reaction zone, a first heat exchanger 2, a second reaction zone, a second heat exchanger 4, and a heating furnace 5;
the first reaction zone is used for enabling a raw material to have an n-butene isomerization reaction in the first reaction zone, and comprises a first reactor 1, wherein the first reactor 1 is provided with an inlet and an outlet; the inlet is connected with the outlet of the heating furnace 5 through a pipeline, and a first valve 6 is arranged on the pipeline; the inlet is also connected with a raw material outlet of the second heat exchanger through a pipeline, and a second valve 7 is arranged on the pipeline; the outlet is connected with the product inlet of the first heat exchanger 2 through a pipeline;
the first heat exchanger 2 is used for exchanging heat between the raw material and the product of the first reactor, and is provided with a raw material inlet, a raw material outlet, a product inlet and a product outlet; the raw material inlets are connected through a pipeline raw material tank (not shown in the figure) for storing reaction raw materials, and a fifth valve 10 is arranged on a pipeline of the raw material tank; the raw material inlet is also connected with the raw material outlet of the second heat exchanger 4 through a pipeline, and a sixth valve 11 is arranged on the pipeline; the raw material outlet is connected with the inlet of the second reactor through a pipeline, and a fourth valve 9 is arranged on the raw material outlet; the raw material outlet is connected with the inlet of the heating furnace 5 through a pipeline, and a seventh valve 12 is arranged on the pipeline; the raw material outlet is also connected with the raw material inlet of the second heat exchanger 4 through a pipeline, and an eighth valve 13 is arranged on the pipeline; the product outlet outputs the first reactor product after heat exchange;
the second reaction zone is used for enabling the raw materials to have n-butene isomerization reaction in the second reaction zone and comprises a second reactor 3, and an inlet and an outlet are arranged on the second reactor 3; the inlet is connected with the outlet of the heating furnace 5 through a pipeline, and a third valve 8 is arranged on the pipeline; the inlet is also connected with the raw material outlet of the first heat exchanger through a pipeline, and a fourth valve 9 is arranged on the pipeline; the outlet is connected with the product inlet of the second heat exchanger 4 through a pipeline;
the second heat exchanger 4 is used for exchanging heat between the raw material and the product of the first reactor, and is provided with a raw material inlet, a raw material outlet, a product inlet and a product outlet; the raw material inlet is connected with a raw material tank (not shown in the figure) through a pipeline, and a ninth valve 14 is arranged on the raw material tank; the raw material inlet is also connected with the raw material outlet of the first heat exchanger 2 through a pipeline, and an eighth valve 13 is arranged on the raw material inlet; the raw material outlet is connected with the inlet of the heating furnace 5 through a pipeline, and a tenth valve 15 is arranged on the pipeline; the raw material outlet is also connected with the raw material inlet of the first heat exchanger 2 through a pipeline, and a sixth valve 11 is arranged on the pipeline; the product outlet outputs the second reactor product after heat exchange;
the heating furnace 5 is used for heating raw materials, an inlet and an outlet are arranged on the heating furnace, the inlet is respectively connected with the raw material outlet of the first heat exchanger 2 and the raw material outlet of the second heat exchanger 4 through pipelines, and the outlet is respectively connected with the inlet of the first reactor 1 and the inlet of the second reactor 3 through pipelines.
Example 1
The isomerization reaction of n-butene was carried out by using the apparatus shown in FIG. 2, and the annual output of the apparatus was 20 ten thousand tons/year.
Firstly, opening a first valve 6, a fifth valve 10 and a seventh valve 12, closing a third valve 8, a fourth valve 9, an eighth valve 13 and a ninth valve 14, starting a first reactor 1, exchanging heat between a first raw material and a product of the first reactor 1 in a first heat exchanger 2, then entering a heating furnace through a raw material outlet of the first heat exchanger 2 to be heated to 290 ℃, and sending the raw material to the first reactor 1 for reaction; the feeding amount of the first raw material is 25 tons/hour; at this time, the product obtained from the first reactor 1 enters the first heat exchanger 2 through the product inlet; when the isomerization conversion of the first reactor is less than 40%, starting to raise the temperature of the first reactor;
when the temperature in the first reactor 1 reached 340 ℃ (approximately 14 days in the process), the temperature of the outlet product was 370 ℃; at this time, the second reactor 3 is started, and the initial reaction temperature in the second reactor 3 is 290 ℃; opening a first valve 6, a fourth valve 9, a sixth valve 11, a ninth valve 14 and a tenth valve 15, closing a second valve 7, a third valve 8, a fifth valve 10, a seventh valve 12 and an eighth valve 13, enabling the first raw material and the second raw material to enter a second heat exchanger 4 to exchange heat with a product of a second reactor 3, enabling the second raw material to enter a first heat exchanger 2, enabling the first raw material to enter a heating furnace 5, controlling the feeding amount of the first raw material to be unchanged through a second flowmeter 17 and a fourth flowmeter 19, enabling the feeding amount of the second raw material to be 15-20 tons/hour, enabling the raw material to be heated to 290 ℃ from room temperature after the second raw material exchanges heat with an outlet product of the first reactor, and enabling the raw material to enter the second reactor 3 to react; heating the first raw material to 340 ℃ through a heating furnace, and reacting in a first reactor 1; adjusting the feeding amount of the second reactor within the range of 15-20 tons/hour according to the temperature of the second reactor 3 to ensure that the temperature of the second reactor 3 can maintain the conversion rate of the structuring reaction to be not less than 40%;
when the reaction temperature in the first reactor rises to 360 ℃, the first reactor 1 is stopped and the catalyst regeneration is carried out (about 7 days in the process); at this time, the third valve 8, the ninth valve 14 and the tenth valve 15 are opened, the first valve 6, the second valve 7, the fifth valve 10 and the sixth valve 11 are closed, the second raw material exchanges heat with the product of the second reactor in the second heat exchanger 4, enters the heating furnace 5 through the raw material outlet of the second heat exchanger 4, is heated to the reaction temperature of the second reactor, and is sent to the second reactor 3 for reaction; meanwhile, the feeding amount of the second raw material is changed to 25 tons/hour;
when the isomerization reaction conversion rate of the second reactor 3 is less than 40%, raising the reaction temperature in the second reactor;
when the reaction temperature in the second reactor 3 is increased to 340 ℃ (about 15 days in the process), the temperature of the outlet product is 370 ℃, the first reactor 1 is started, and the initial reaction temperature in the first reactor is 290 ℃; opening a second valve 7, a third valve 8, a fifth valve 10, a seventh valve 12 and an eighth valve 13, closing a first valve 6, a fourth valve 9, a sixth valve 11, a ninth valve 14 and a tenth valve 15, enabling the first raw material and the second raw material to enter a first heat exchanger 2 to exchange heat with a product of a first reactor 1, enabling the first raw material to enter a second heat exchanger 4, heating the raw materials from room temperature to 290 ℃, and enabling the raw materials to enter the first reactor 1 for reaction; the second raw material enters a heating furnace 5, is heated to 340 ℃ by the heating furnace and enters a second reactor 3; controlling the feeding amount of the second raw material to be constant through the first flow meter 16 and the third flow meter 18, and controlling the feeding amount of the first raw material to be 15-20 tons/hour; adjusting the feeding amount of the first reactor within the range of 15-20 tons/hour according to the temperature of the first reactor 1 to ensure that the temperature of the first reactor 1 can maintain the conversion rate of the structuring reaction to be not less than 40%;
when the reaction temperature in the second reactor 3 rises to 360 ℃, the second reactor 3 is stopped and the catalyst regeneration is carried out (about 7 days in the process); opening a first valve 6, a fifth valve 10 and a seventh valve 12, closing a third valve 8, a fourth valve 9, an eighth valve 13 and a ninth valve 14, starting the first reactor 1, exchanging heat between a first raw material and a product of the first reactor 1 in a first heat exchanger 2, then entering a heating furnace through a raw material outlet of the first heat exchanger 2 to be heated to 290 ℃, and sending the heated raw material to the first reactor for reaction; meanwhile, the feeding amount of the first raw material is changed to 25 tons/hour; when the isomerization conversion in the first reactor 1 is less than 40%, the temperature of the first reactor 1 is started to be raised and the above operation is repeated.
By adopting the device and the method, the equipment is operated only 50% of the time per year, and the operation is improved to 70% of the time per year, so that the yield of isobutene can be increased by 70-80%, and the utilization rate of the catalyst and the equipment can be increased by 70-80%.
Any numerical value mentioned in this specification, if there is only a two unit interval between any lowest value and any highest value, includes all values from the lowest value to the highest value incremented by one unit at a time. For example, if it is stated that the amount of a component, or a value of a process variable such as temperature, pressure, time, etc., is 50 to 90, it is meant in this specification that values of 51 to 89, 52 to 88 … …, and 69 to 71, and 70 to 71, etc., are specifically enumerated. For non-integer values, units of 0.1, 0.01, 0.001, or 0.0001 may be considered as appropriate. These are only some specifically named examples. In a similar manner, all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be disclosed in this application.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (14)
1. A method of isomerizing n-butenes comprising:
s1, sending the first raw material to a first reaction area for reaction, wherein the initial reaction temperature in the first reaction area is 290-300 ℃;
s2, when the isomerization reaction conversion rate in the first reaction zone is lower than 40%, increasing the reaction temperature of the first reaction zone;
s3, when the reaction temperature in the first reaction zone is increased to 335-; meanwhile, the first raw material and the product flow of the second reaction zone exchange heat, and then are heated to 335-;
s4, when the reaction temperature in the first reaction zone rises to 355-365 ℃, stopping the reaction in the first reaction zone, regenerating the catalyst in the first reaction zone, and sending the second raw material to the second reaction zone for reaction;
s5, when the isomerization reaction conversion rate in the second reaction zone is lower than 40%, increasing the reaction temperature in the second reaction zone;
s6, when the reaction temperature in the second reaction zone is increased to 335-; meanwhile, the second raw material exchanges heat with the product flow in the first reaction zone, and then is heated to 335-;
s7, when the reaction temperature in the second reaction area rises to 355-365 ℃, stopping the reaction in the second reaction area, regenerating the catalyst in the second reaction area, and sending the first raw material to the first reaction area for reaction;
s8 repeats steps S2-S7.
2. The method of claim 1, wherein in step S1, the first raw material is first heat exchanged with the product stream of the first reaction zone, then heated to the reaction temperature of the first reaction zone, and sent to the first reaction zone for reaction.
3. The method of claim 1 or 2, wherein in step S3, the feeding amount of the second reaction zone is adjusted according to the reaction temperature in the second reaction zone, so as to ensure that the reaction temperature in the second reaction zone is not lower than 290 ℃.
4. The method according to claim 1 or 2, wherein in step S3, the feeding amount of the second raw material is adjusted according to the reaction temperature in the second reaction zone, and the feeding amount of the second raw material is 60 to 80% of the feeding amount of the first raw material.
5. The method as claimed in claim 1 or 2, wherein the temperature of the second raw material after heat exchange with the product streams of the second reaction zone and the first reaction zone in sequence in step S3 is 290-300 ℃.
6. The method of claim 1 or 2, wherein in step S4, the second raw material is first heat exchanged with the product stream of the second reaction zone, and then heated by the heating furnace to the reaction temperature of the second reaction zone, and sent to the second reaction zone for reaction.
7. The method of claim 1 or 2, wherein in step S6, the feeding amount of the first reaction zone is adjusted according to the reaction temperature in the first reaction zone, so as to ensure that the reaction temperature in the first reaction zone is not lower than 290 ℃.
8. The method of claim 1 or 2, wherein in step S6, the feeding amount of the first raw material is adjusted according to the reaction temperature in the first reaction zone, and the feeding amount of the first raw material is 60-80% of the feeding amount of the second raw material.
9. The method as claimed in claim 1 or 2, wherein the temperature of the first raw material after heat exchange with the product streams of the first reaction zone and the second reaction zone in sequence in step S6 is 290-300 ℃.
10. The process of claim 1 or 2, wherein the feedstock comprises n-butenes and a catalyst; and/or the catalyst comprises a ZSM-35 molecular sieve, the silica-alumina ratio of the catalyst is 40-60, and the regeneration period is more than 40 days.
11. An apparatus for the isomerization of n-butenes, comprising:
the reactor of the first reaction zone is provided with an inlet and an outlet, the inlet is respectively connected with the outlet of the heating furnace and the raw material outlet of the second heat exchanger, and the outlet is connected with the product inlet of the first heat exchanger;
the first heat exchanger is used for exchanging heat between the raw material and the product of the first reaction zone reactor, and is provided with a raw material inlet, a raw material outlet, a product inlet and a product outlet, wherein the raw material inlet is respectively connected with the raw material tank and the raw material outlet of the second heat exchanger, the raw material outlet is respectively connected with the inlet of the heating furnace, the raw material inlet of the second heat exchanger and the inlet of the second reaction zone reactor, and the product outlet outputs a product flow obtained by the first reaction zone;
the second reaction zone is used for enabling the raw materials to have n-butene isomerization reaction in the second reaction zone, an inlet and an outlet are arranged on a reactor of the second reaction zone, the inlet is respectively connected with an outlet of the heating furnace and a raw material outlet of the first heat exchanger, and the outlet is connected with a product inlet of the second heat exchanger;
the second heat exchanger is used for exchanging heat between the raw material and the product of the second reaction zone reactor, and is provided with a raw material inlet, a raw material outlet, a product inlet and a product outlet, wherein the raw material inlet is respectively connected with the raw material tank and the raw material outlet of the first heat exchanger, the raw material outlet is respectively connected with the inlet of the heating furnace, the raw material inlet of the first heat exchanger and the inlet of the first reaction zone reactor, and the product outlet outputs the product obtained by the second reaction zone reactor;
the heating furnace is used for heating raw materials, an inlet and an outlet are arranged on the heating furnace, the inlet is respectively connected with the raw material outlet of the first heat exchanger and the raw material outlet of the second heat exchanger, and the outlet is respectively connected with the inlet of the first reaction zone reactor and the inlet of the second reaction zone reactor;
and the pipeline is used for connecting the devices and is provided with a valve.
12. The apparatus of claim 11, wherein a feed channel and a product channel are provided within the first heat exchanger, respectively; the raw material channel is respectively communicated with a raw material inlet and a raw material outlet and is used for circulating the raw material entering the first heat exchanger; the product channel is in communication with the product inlet and the product outlet, respectively, for circulating a product stream into the first heat exchanger.
13. The apparatus of claim 11 or 12, wherein a feed channel and a product channel are provided in the second heat exchanger, respectively; the raw material channel is respectively communicated with the raw material inlet and the raw material outlet and is used for circulating the raw material entering the second heat exchanger; the product channel is in communication with the product inlet and the product outlet, respectively, for circulating a product stream into the second heat exchanger.
14. Use of the apparatus according to any one of claims 11 to 13 for the isomerization of n-butenes.
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