CN220634258U - Production system of N-methyl pyrrolidone - Google Patents

Production system of N-methyl pyrrolidone Download PDF

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Publication number
CN220634258U
CN220634258U CN202322169185.6U CN202322169185U CN220634258U CN 220634258 U CN220634258 U CN 220634258U CN 202322169185 U CN202322169185 U CN 202322169185U CN 220634258 U CN220634258 U CN 220634258U
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outlet
synthesizing device
methylamine
methylpyrrolidone
self
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顾朝晖
张少利
袁红玲
李庆华
耍芬芬
朱止阳
申长皓
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Henan Xinlianxin Chemicals Group Co Ltd
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Henan Xinlianxin Chemicals Group Co Ltd
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Abstract

The utility model relates to a production system of N-methyl pyrrolidone; the device comprises a 1, 4-butanediol storage tank, wherein the 1, 4-butanediol storage tank is connected with a gamma-butyrolactone synthesizing device, a gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device is connected with an inlet of an N-methylpyrrolidone synthesizing device, a hydrogen outlet of the gamma-butyrolactone synthesizing device is connected with a gas pretreatment unit and an ammonia synthesizing device, a liquid ammonia outlet of the ammonia synthesizing device is connected with a methylamine synthesizing device, an outlet of the methylamine synthesizing device is connected with a methylamine rectifying device, and a monomethylamine outlet of the methylamine rectifying device is connected with an inlet of the N-methylpyrrolidone synthesizing device; the method has the advantages of effectively utilizing byproduct hydrogen, reducing tail gas treatment investment, reducing the external production cost of raw material liquid ammonia, reducing the raw material cost for producing N-methyl pyrrolidone and enhancing the cost competitiveness of enterprises.

Description

Production system of N-methyl pyrrolidone
Technical Field
The utility model belongs to the field of N-methyl pyrrolidone production equipment, and particularly relates to a production system of N-methyl pyrrolidone.
Background
NMP (N-methyl pyrrolidone) is an important organic chemical raw material, and NMP products are widely applied to industries such as lithium batteries, medicines, pigments, cleaning agents, insulating materials and the like. At present, the main production and application are concentrated in the fields of lithium ion batteries, electric automobile power batteries, para-aramid fibers and the like. The polyurethane resin can be widely applied to perfumes and medical intermediates, can be used as a carrier in polymerization reaction and participate in the polymerization reaction, and is also commonly used as a solvent of resin and a viscosity modifier of polyurethane.
NMP is mainly synthesized by gamma-butyrolactone (GBL) and monomethylamine as raw materials, and in order to reduce the purchase cost of gamma-butyrolactone, some enterprises adopt the form of producing GBL internally, and the GBL synthesis method mainly comprises the following three types according to raw material classification: the method comprises a furfural method, a maleic anhydride hydrogenation method and a 1, 4-Butanediol (BDO) dehydrogenation method, wherein the furfural method has a complex process, so that the generation cost is relatively high, and the method is not generally used in China at present; maleic anhydride hydrogenation method is limited by domestic and foreign raw materials, and related equipment is not stolen in China; the 1, 4-Butanediol (BDO) dehydrogenation method is popular in most enterprises because of sufficient raw material sources and mature and stable process technology; but the 1, 4-Butanediol (BDO) dehydrogenation method is actually carried outA large amount of hydrogen is generated in the running process, which definitely causes the waste of gas resources; for example: chinese patent CN203295405U discloses a dehydrogenation reaction device for preparing GBL by butanediol, which solves the problem that GBL prepared by BDO dehydrogenation cannot be continuously produced, but refines the product and produces byproduct H 2 The treatment measures are not explained. Specifically, about 530Nm by-product per ton of GBL produced 3 H of (2) 2 The larger the device is, the larger the byproduct H 2 The more H 2 As valuable effective gas resources in the chemical industry, how to use the effective gas resources becomes a problem to be solved urgently for enterprises.
Disclosure of Invention
The utility model aims to provide a production system of N-methyl pyrrolidone, which solves the problems in the background art.
In order to achieve the above purpose, the present utility model provides the following technical solutions:
the production system of the N-methylpyrrolidone comprises a 1, 4-butanediol storage tank, wherein the 1, 4-butanediol storage tank is connected with a gamma-butyrolactone synthesizing device, a gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device is connected with an inlet of the N-methylpyrrolidone synthesizing device, a hydrogen outlet of the gamma-butyrolactone synthesizing device is connected with a gas pretreatment unit and an ammonia synthesizing device, a liquid ammonia outlet of the ammonia synthesizing device is connected with a methylamine synthesizing device, an outlet of the methylamine synthesizing device is connected with a methylamine rectifying device, and a monomethylamine outlet of the methylamine rectifying device is connected with an inlet of the N-methylpyrrolidone synthesizing device.
The beneficial effects of the utility model are as follows: based on the existing N-methyl pyrrolidone synthesis method, the hydrogen generated by dehydrogenation is coupled with an ammonia synthesis device in the coal chemical industry and is used for producing liquid ammonia; and the liquid ammonia is matched with the methanol to be used for producing the monomethylamine, so that the effective utilization of effective gas resources is realized on the premise of reducing the cost of purchasing the monomethylamine by enterprises.
Preferably, the outlet of the N-methylpyrrolidone synthesis device is connected with the N-methylpyrrolidone rectification device through a seventh self-regulating valve, and the product outlet of the N-methylpyrrolidone rectification device is connected with the N-methylpyrrolidone storage tank.
Preferably, the gas pretreatment unit comprises a pressure swing adsorption hydrogen extracting device connected with a hydrogen outlet of the gamma-butyrolactone synthesizing device, an outlet of the pressure swing adsorption hydrogen extracting device is connected with a synthesis gas compressor, and an inlet of the synthesis gas compressor is also connected with a nitrogen outlet of the air separation device through a tenth self-regulating valve.
Preferably, the inlet of the methylamine synthesis device is connected with the outlets of the liquid ammonia storage tank and the methanol storage tank respectively, and the liquid ammonia storage tank is connected with the liquid ammonia outlet of the ammonia synthesis device through a twelfth self-regulating valve.
Preferably, a fifth self-regulating valve is arranged between the 1, 4-butanediol storage tank and the gamma-butyrolactone synthesizing device, a sixth self-regulating valve is arranged between a gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device and an inlet of the N-methylpyrrolidone synthesizing device, an eighth self-regulating valve is arranged between a hydrogen outlet of the gamma-butyrolactone synthesizing device and the pressure swing adsorption hydrogen extracting device, a ninth self-regulating valve is arranged between the pressure swing adsorption hydrogen extracting device and the synthesis gas compressor, and an outlet of the synthesis gas compressor is connected with an inlet of the ammonia synthesizing device through the eleventh self-regulating valve.
Preferably, a third self-regulating valve is arranged between the outlet of the methylamine synthesizing device and the methylamine rectifying device, and a fourth self-regulating valve is arranged between the monomethylamine outlet of the methylamine rectifying device and the inlet of the N-methylpyrrolidone synthesizing device.
Preferably, a first self-regulating valve is arranged between the liquid ammonia storage tank and the inlet of the methylamine synthesizing device, and a second self-regulating valve is arranged between the methanol storage tank and the inlet of the methylamine synthesizing device.
According to the production system of the N-methylpyrrolidone, the existing N-methylpyrrolidone synthesis method is used as a basis, hydrogen generated by dehydrogenation is coupled with an ammonia synthesis device in coal chemical industry, nitrogen from air separation is matched for preparing liquid ammonia, the liquid ammonia and methanol are used as raw materials for producing methylamine, the preparation of monomethylamine which is another raw material for producing the N-methylpyrrolidone is realized through rectification of the methylamine, the cost of purchasing monomethylamine outside enterprises can be reduced when the N-methylpyrrolidone is produced, and meanwhile, hydrogen which is a byproduct of a 1, 4-Butanediol (BDO) dehydrogenation method can be effectively utilized, so that the utilization of effective gas resources is realized; the utility model accords with the characteristics of more coal, less oil and less gas in China through the coupling of hydrogen and a coal chemical device in the gamma-butyrolactone synthesis process, and can realize the stable operation of a system through the design of corresponding self-regulating valves, especially the quantity of monomethylamine in the generated methylamine can be controlled through the arrangement of the first self-regulating valve and the second self-regulating valve, so as to achieve the aim of improving the yield of N-methylpyrrolidone.
Drawings
Fig. 1 is a schematic structural view of the present utility model.
In the figure: 1. a liquid ammonia storage tank; 2. a methanol storage tank; 3. a methylamine synthesis device; 4. methylamine rectifying device; 5. 1, 4-butanediol storage tank; 6. a gamma-butyrolactone synthesizing device; 7. an N-methylpyrrolidone synthesis device; 8. an N-methylpyrrolidone rectifying device; 9. a pressure swing adsorption hydrogen extracting device; 10. an air separation device; 11. a synthesis gas compressor; 12. an ammonia synthesis device; 13. a first self-regulating valve; 14. a second self-regulating valve; 15. a third self-regulating valve; 16. a fourth self-regulating valve; 17. a fifth self-regulating valve; 18. a sixth self-regulating valve; 19. a seventh self-regulating valve; 20. eighth self-regulating valve; 21. a ninth self-regulating valve; 22. a tenth self-regulating valve; 23. an eleventh self-regulating valve; 24. a twelfth self-regulating valve; 25. n-methyl pyrrolidone storage tank.
Detailed Description
The technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model.
Referring to fig. 1, a system for producing N-methylpyrrolidone, comprising a 1, 4-butanediol storage tank 5, wherein the 1, 4-butanediol storage tank 5 is connected with a gamma-butyrolactone synthesizing device 6, a gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device 6 is connected with an inlet of an N-methylpyrrolidone synthesizing device 7, a hydrogen outlet of the gamma-butyrolactone synthesizing device 6 is connected with a gas pretreatment unit and an ammonia synthesizing device 12, a liquid ammonia outlet of the ammonia synthesizing device 12 is connected with a methylamine synthesizing device 3, an outlet of the methylamine synthesizing device 3 is connected with a methylamine rectifying device 4, and a monomethylamine outlet of the methylamine rectifying device 4 is connected with an inlet of the N-methylpyrrolidone synthesizing device 7. The gamma-butyrolactone synthesizing device 6 consists of a special jacket type reactor and a heat exchanger, the ammonia synthesizing device 12 consists of a special ammonia synthesizing tower, a heat exchanger and the like, the methylamine synthesizing device 3 mainly consists of a tubular methylamine reactor and the heat exchanger, and the methylamine rectifying device 4 consists of tray towers with different heights, and the conventional arrangement is adopted, so that the structure is not repeated. The utility model is based on the existing N-methyl pyrrolidone synthesis method, and the hydrogen generated by dehydrogenation is coupled with an ammonia synthesis device in the coal chemical industry and is used for producing liquid ammonia; and the liquid ammonia is matched with the methanol to be used for producing the monomethylamine, so that the effective utilization of effective gas resources is realized on the premise of reducing the cost of purchasing the monomethylamine by enterprises.
Further, the outlet of the N-methylpyrrolidone synthesis device 7 is connected with the N-methylpyrrolidone rectification device 8 through a seventh self-regulating valve 19, and the product outlet of the N-methylpyrrolidone rectification device 8 is connected with the N-methylpyrrolidone storage tank 25. The N-methyl pyrrolidone synthesizing device 7 consists of a special jacket type reactor and a heat exchanger, and the N-methyl pyrrolidone rectifying device 8 consists of a light component removing tower, a heavy component removing tower and a product refining plate tower, which are arranged conventionally, so that the structure is not repeated. Through the arrangement, the N-methyl pyrrolidone can be proposed, and then the selling is convenient.
Further, the gas pretreatment unit comprises a pressure swing adsorption hydrogen extracting device 9 connected with a hydrogen outlet of the gamma-butyrolactone synthesizing device 6, an outlet of the pressure swing adsorption hydrogen extracting device 9 is connected with a synthesis gas compressor 11, and an inlet of the synthesis gas compressor 11 is also connected with a nitrogen outlet of the air separation device 10 through a tenth self-regulating valve 22. The pressure swing adsorption hydrogen extracting device 9 consists of a plurality of pressure swing adsorption towers, a desorption gas buffer tank, a mixing tank and a plurality of program control valves and manual valves; the air separation device 10 is composed of advanced cryogenic separation equipment and components, and adopts the processes of purifying air by molecular sieve, pressurizing air, refrigerating by a pressurizing turbine expander and compressing oxygen to separate high-purity N 2 The method comprises the steps of carrying out a first treatment on the surface of the The above is a conventional arrangement, and therefore the structure is not repeated. By the arrangement, the synthesis of gamma-butyrolactone can be utilizedThe hydrogen removed in unit 6 is used as a feedstock and is combined with high purity N from air separation unit 10 2 Can be used as raw materials for producing liquid ammonia together so as to achieve the purpose of improving the utilization rate of hydrogen.
Further, the inlet of the methylamine synthesizing device 3 is respectively connected with the outlets of the liquid ammonia storage tank 1 and the methanol storage tank 2, and the liquid ammonia storage tank 1 is connected with the liquid ammonia outlet of the ammonia synthesizing device 12 through a twelfth self-regulating valve 24; a third self-regulating valve 15 is arranged between the outlet of the methylamine synthesizing device 3 and the methylamine rectifying device 4, and a fourth self-regulating valve 16 is arranged between the monomethylamine outlet of the methylamine rectifying device 4 and the inlet of the N-methylpyrrolidone synthesizing device 7. By the arrangement, the liquid ammonia and the methanol produced by the method can be used as raw materials for producing the methylamine, and the methylamine is produced by the methylamine rectifying device 4 and used as raw materials for synthesizing and producing the N-methylpyrrolidone.
Further, a fifth self-regulating valve 17 is arranged between the 1, 4-butanediol storage tank 5 and the gamma-butyrolactone synthesizing device 6, a sixth self-regulating valve 18 is arranged between the gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device 6 and the inlet of the N-methylpyrrolidone synthesizing device 7, an eighth self-regulating valve 20 is arranged between the hydrogen outlet of the gamma-butyrolactone synthesizing device 6 and the pressure swing adsorption hydrogen extracting device 9, a ninth self-regulating valve 21 is arranged between the pressure swing adsorption hydrogen extracting device 9 and the synthetic gas compressor 11, and the outlet of the synthetic gas compressor 11 is connected with the inlet of the ammonia synthesizing device 12 through the eleventh self-regulating valve 23.
Further, a third self-regulating valve 15 is arranged between the outlet of the methylamine synthesizing device 3 and the methylamine rectifying device 4, and a fourth self-regulating valve 16 is arranged between the monomethylamine outlet of the methylamine rectifying device 4 and the inlet of the N-methylpyrrolidone synthesizing device 7.
Further, a first self-regulating valve 13 is arranged between the liquid ammonia storage tank 1 and the inlet of the methylamine synthesizing device 3, and a second self-regulating valve 14 is arranged between the methanol storage tank 2 and the inlet of the methylamine synthesizing device 3.
The working principle of the utility model is as follows: the liquid ammonia raw material from the liquid ammonia storage tank 1 enters the methylamine synthesizing device 3 through the first self-adjusting valve 13, the methanol raw material from the methanol storage tank 2 enters the methylamine synthesizing device 3 through the second self-adjusting valve 14, and the liquid ammonia raw material and the methanol raw material are mixed with each otherSynthesizing mixed methylamine in the methanol storage tank 2, wherein the mixed methylamine comprises monomethylamine, dimethylamine and trimethylamine, and the proportion of the monomethylamine, the dimethylamine and the trimethylamine in the mixed methylamine can be controlled through the first self-regulating valve 13 and the second self-regulating valve 14 so as to realize the improvement of the monomethylamine; the mixed methylamine is rectified by a methylamine rectifying device 4, and the monomethylamine separated by rectification enters an N-methylpyrrolidone synthesizing device 7 through a fourth self-regulating valve; the 1, 4-butanediol in the 1, 4-butanediol storage tank 5 enters a gamma-butyrolactone synthesizing device 6, the gamma-butyrolactone synthesizing device 6 is specifically a device for preparing gamma-butyrolactone by dehydrogenating 1, 4-butanediol, a gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device 6 enters an N-methylpyrrolidone synthesizing device 7 through a sixth self-regulating valve 18, the proportion of monomethylamine and gamma-butyrolactone can be regulated through the sixth self-regulating valve 18 and a fourth self-regulating valve 16, and after N-methylpyrrolidone synthesized by the N-methylpyrrolidone synthesizing device 7 is rectified by an N-methylpyrrolidone rectifying device, a product is sent into an N-methylpyrrolidone storage tank 25 through a pipeline; h coming out of the gamma-butyrolactone synthesizing apparatus 6 2 The purified hydrogen enters the pressure swing adsorption hydrogen extraction device 9 through the eighth self-regulating valve 20, enters the synthesis gas compressor 11 through the ninth self-regulating valve 21, and the high-purity nitrogen in the air separation device 10 enters the synthesis gas compressor 11 according to a certain proportion through the tenth self-regulating valve; the synthesis gas compressor 11 compresses the above-mentioned gas, and the compressed synthesis gas is fed into the ammonia synthesis device 12 through eleventh self-regulating valve 23, and the liquid ammonia produced in the above-mentioned ammonia synthesis device 12 is fed into the liquid ammonia storage tank 1 through twelfth self-regulating valve 24 as raw material for producing monomethylamine. The operating temperature of the methylamine synthesis device 3 in the above process is: 400-430 ℃, the pressure is: 2.4MPa to 2.6MPa, and the operation temperature of the methylamine rectifying device 4 is as follows: 45-150 ℃, the pressure is: 0.85-1.85 MPa; the operating temperature of the BDO dehydrogenation GBL manufacturing device 6 is as follows: 60-250 ℃, the pressure is: -0.06MPa to 1.2MPa; the operating temperature of the NMP synthesis unit 7 is: 100-280 ℃, the pressure is: 7.0MPa to 9.0MPa, and the operating temperature of the NMP refining device 8 is as follows: 100-150 ℃, the pressure is: -0.06MPa to 1.2MPa; the operating temperature of the PSA hydrogen-extracting device 9 is as follows: 20-45 ℃,the pressure is: 0.1MPa to 4.5MPa; operating temperature of the synthesis gas compression unit 11: 30-100 ℃, pressure: 4.0MPa to 15.0MPa, and the operating temperature of the ammonia synthesis device 12 is as follows: 470-490 ℃ and the pressure is as follows: 17.0MPa to 18.0MPa. The utility model utilizes BDO dehydrogenation device to obtain products GBL and H 2 By-product H 2 High-purity H can be obtained after purification by the pressure swing adsorption hydrogen extracting device 9 2 ,H 2 Preparing liquid ammonia as a raw material of synthetic ammonia, and preparing methylamine by coupling the liquid ammonia as a raw material of a methylamine device; the method not only effectively utilizes the byproduct hydrogen and reduces the tail gas treatment investment, but also reduces the external production cost of raw material liquid ammonia, reduces the raw material cost of each device and enhances the cost competitiveness of enterprises.
Although embodiments of the present utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A production system of N-methylpyrrolidone, comprising a 1, 4-butanediol storage tank (5), characterized in that: the 1, 4-butanediol storage tank (5) is connected with the gamma-butyrolactone synthesizing device (6), the gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device (6) is connected with the inlet of the N-methylpyrrolidone synthesizing device (7), the hydrogen outlet of the gamma-butyrolactone synthesizing device (6) is connected with the gas pretreatment unit and the ammonia synthesizing device (12), the liquid ammonia outlet of the ammonia synthesizing device (12) is connected with the methylamine synthesizing device (3), the outlet of the methylamine synthesizing device (3) is connected with the methylamine rectifying device (4), and the monomethylamine outlet of the methylamine rectifying device (4) is connected with the inlet of the N-methylpyrrolidone synthesizing device (7).
2. A system for producing N-methylpyrrolidone according to claim 1, characterized in that: the outlet of the N-methylpyrrolidone synthesis device (7) is connected with the N-methylpyrrolidone rectification device (8) through a seventh self-regulating valve (19), and the product outlet of the N-methylpyrrolidone rectification device (8) is connected with the N-methylpyrrolidone storage tank (25).
3. A system for producing N-methylpyrrolidone according to claim 1, characterized in that: the gas pretreatment unit comprises a pressure swing adsorption hydrogen extracting device (9) connected with a hydrogen outlet of the gamma-butyrolactone synthesizing device (6), an outlet of the pressure swing adsorption hydrogen extracting device (9) is connected with a synthesis gas compressor (11), and an inlet of the synthesis gas compressor (11) is also connected with a nitrogen outlet of the air separation device (10) through a tenth self-regulating valve (22).
4. A system for producing N-methylpyrrolidone according to claim 1, characterized in that: the inlet of the methylamine synthesis device (3) is respectively connected with the outlets of the liquid ammonia storage tank (1) and the methanol storage tank (2), and the liquid ammonia storage tank (1) is connected with the liquid ammonia outlet of the ammonia synthesis device (12) through a twelfth self-regulating valve (24).
5. A system for producing N-methylpyrrolidone according to claim 3, characterized in that: a fifth self-regulating valve (17) is arranged between the 1, 4-butanediol storage tank (5) and the gamma-butyrolactone synthesizing device (6), a sixth self-regulating valve (18) is arranged between a gamma-butyrolactone outlet of the gamma-butyrolactone synthesizing device (6) and an inlet of the N-methylpyrrolidone synthesizing device (7), an eighth self-regulating valve (20) is arranged between a hydrogen outlet of the gamma-butyrolactone synthesizing device (6) and the pressure swing adsorption hydrogen extracting device (9), a ninth self-regulating valve (21) is arranged between the pressure swing adsorption hydrogen extracting device (9) and the synthetic gas compressor (11), and an outlet of the synthetic gas compressor (11) is connected with an inlet of the ammonia synthesizing device (12) through an eleventh self-regulating valve (23).
6. A system for producing N-methylpyrrolidone according to claim 1, characterized in that: a third self-regulating valve (15) is arranged between the outlet of the methylamine synthesizing device (3) and the methylamine rectifying device (4), and a fourth self-regulating valve (16) is arranged between the monomethylamine outlet of the methylamine rectifying device (4) and the inlet of the N-methylpyrrolidone synthesizing device (7).
7. The system for producing N-methylpyrrolidone according to claim 4, wherein: a first self-regulating valve (13) is arranged between the liquid ammonia storage tank (1) and the inlet of the methylamine synthesizing device (3), and a second self-regulating valve (14) is arranged between the methanol storage tank (2) and the inlet of the methylamine synthesizing device (3).
CN202322169185.6U 2023-08-11 2023-08-11 Production system of N-methyl pyrrolidone Active CN220634258U (en)

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