CN108129330B - Cyclopropylamine continuous production system and production method - Google Patents
Cyclopropylamine continuous production system and production method Download PDFInfo
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- CN108129330B CN108129330B CN201711492500.1A CN201711492500A CN108129330B CN 108129330 B CN108129330 B CN 108129330B CN 201711492500 A CN201711492500 A CN 201711492500A CN 108129330 B CN108129330 B CN 108129330B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/54—Preparation of compounds containing amino groups bound to a carbon skeleton by rearrangement reactions
- C07C209/58—Preparation of compounds containing amino groups bound to a carbon skeleton by rearrangement reactions from or via amides
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- C07—ORGANIC CHEMISTRY
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- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
Abstract
The invention belongs to the field of chemical production, and particularly relates to a continuous production system and a continuous production method for cyclopropylamine. The cyclopropylamine continuous production system comprises the following production devices which are connected in sequence: a first-stage reaction distillation kettle, a second-stage reaction distillation kettle, an ammoniation reactor, an ammonia removal tank, a flash tank, a methanol removal tower, a phase separator and a degradation reactor. The invention relates to a method for producing cyclopropylamine by using the cyclopropylamine continuous production system, which solves the problem of intermittent production of the prior cyclopropylamine; the material fluidity and filterability in the cyclization, ammoniation and ammoniation distillation processes are improved; improves the degradation process of the cyclopropylcarboxamide, ensures the achievement of high conversion rate and high yield of the cyclopropylamine, and realizes the continuous production of the cyclopropylamine.
Description
Technical Field
The invention belongs to the field of chemical production, and particularly relates to a continuous production system and a continuous production method for cyclopropylamine.
Background
Cyclopropylamine (CPA) is a three-membered ring aliphatic amine, belongs to an important medical intermediate, is widely applied to the fields of medicines, pesticides and the like, can be used for synthesizing antibacterial drugs such as ciprofloxacin, enrofloxacin, sparfloxacin and the like, and can also be used for preparing chemical herbicides such as propisochlor, ciprofloxacin and the like.
One of the current methods for factory production of cyclopropylamine is: methyl chlorobutyrate is adopted as a raw material, cyclization reaction is carried out on the methyl chlorobutyrate and sodium methoxide to generate methyl cyclopropanecarboxylate, the methyl cyclopropanecarboxylate is aminated at medium temperature and medium pressure to generate cyclopropanecarboxamide (CPCA), and the cyclopropanecarboxamide is aminated and distilled to carry out Hofmann degradation on the cyclopropanecarboxamide and sodium hypochlorite to obtain cyclopropylamine.
In industry, due to various technical problems, the whole production flow of cyclopropylamine is operated intermittently, and continuous production is not realized. The prior intermittent production system and reaction conditions of the cyclopropylamine are as follows:
the device in the existing cyclopropylamine batch production system mainly comprises: the device comprises a cyclization reaction kettle, a high-pressure ammoniation reaction kettle, a methanol xylene distillation kettle, a cyclopropanecarboxamide degradation reaction kettle, a pre-distillation kettle for crude distillation, a cyclopropylamine crude distillation kettle and a cyclopropylamine rectification kettle, wherein the devices are required to be operated intermittently. Firstly, carrying out cyclization reaction on sodium methoxide and methyl chlorobutyrate in a cyclization reaction kettle to generate methyl cyclopropanecarboxylate, then sending the material to a high-pressure ammonification reaction kettle, adding liquid ammonia into the high-pressure ammonification reaction kettle to carry out ammonification reaction, then transferring the material to a methanol xylene distillation kettle, distilling until the material in the kettle is semisolid, adding water, and sending a water layer to a degradation reaction kettle of the cyclopropanecarboxamide; adding alkali liquor and sodium hypochlorite solution into a cyclopropanecarboxamide degradation kettle for degradation reaction, then transferring the material to a pre-distillation kettle for crude distillation, operating a cyclopropylamine crude distillation kettle and a cyclopropylamine distillation kettle, and rectifying to obtain a cyclopropylamine product.
In the first step of the cyclization, a large amount of NaCl is formed, and the presence of salts in the organic phase (such as xylene) increases the viscosity of the reaction solution, reduces the fluidity thereof, and causes inconvenience and variability in continuous production. The solubility of the cyclopropanecarboxamide formed in the second amination step in a solvent (e.g., xylene) is low, so that the cyclopropanecarboxamide is precipitated at a low temperature, and the fluidity of the reaction solution becomes worse. The third step of Hofmann degradation is the last reaction of the prior common production process of Cyclopropylamine (CPA), and is also a link with relatively low yield and more variables. The hofmann degradation process actually involves three stages, substitution, elimination (rearrangement) and hydrolysis, or two stages, chlorination and decarbonization (the rearrangement product is very hydrolyzed, so the elimination and hydrolysis stages can be combined to be referred to as the "decarbonization" stage). In the Hofmann degradation process, two side reactions have important influence on the yield of CPA, one is hydrolysis products (such as carbon dioxide) of the cyclopropane carboxamide (CPCA), and the other is excessive sodium hypochlorite which oxidizes raw materials, intermediate products and target products to generate impurities such as nitrile and the like. The content of alkali in the solution, the reaction temperature and the addition amount of effective chlorine have different degrees of influence on three stages in the Hofmann degradation process, so that the reaction yield has great variables, and a lot of problems are brought to the realization of continuous operation.
Heretofore, due to the various technical problems, the industrial production of cyclopropylamine adopts an intermittent operation process, which has low production efficiency, low and unstable product yield and has a lot of promotion space.
Therefore, the development of a system and a method for continuously producing cyclopropylamine is of great significance for improving the production efficiency and the product yield.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a continuous production system for cyclopropylamine. The production system can be used for continuously producing the cyclopropylamine.
In order to achieve the above object, the present invention provides a continuous production system for cyclopropylamine, comprising the following production apparatuses connected in sequence: a first-stage reaction distillation kettle, a second-stage reaction distillation kettle, an ammoniation reactor, an ammonia removal tank, a flash tank, a methanol removal tower, a phase separator and a degradation reactor.
Wherein, the ammoniation reactor is a kettle type ammoniation reactor or a tubular ammoniation reactor. Preferably a tubular ammoniation reactor.
Wherein, the degradation reactor is a kettle-type degradation reactor or a tubular degradation reactor, and preferably a tubular degradation reactor.
The continuous production system of the cyclopropylamine provided by the invention also comprises a continuous crude distillation tower and a continuous fine distillation tower after the degradation reactor.
The continuous production system for the cyclopropylamine provided by the invention further comprises a pipeline, a control instrument and a control device, wherein the pipeline is connected with each production device. The automatic Control System adopts a Control technology mainly including a Distributed Control System (DCS).
Wherein, the accessories are heat supply, cold supply, safety and the like.
Another objective of the present invention is to provide a continuous production method of cyclopropylamine, which utilizes the continuous production system of cyclopropylamine, comprising:
step a), continuously feeding methyl chlorobutyrate, sodium methoxide and a solvent into a primary reaction distillation kettle, carrying out cyclization reaction on the methyl chlorobutyrate and the sodium methoxide to generate methyl cyclopropanecarboxylate, continuously distilling out methanol in the reaction process, feeding a kettle bottom product of the primary reaction distillation kettle into a secondary reaction distillation kettle for further reaction and distilling the methanol;
step b) methanol distilled from the first-stage reaction distillation kettle and the second-stage reaction distillation kettle, and materials and NH discharged from the second-stage reaction distillation kettle3Mixing the mixture with methyl cyclopropanecarboxylate and NH in an ammoniation reactor3Performing ammoniation reaction to generate the cyclopropanecarboxamide, and enabling the reaction material to enter an ammonia removal tank, a flash tank and a methanol removal tower to remove NH after coming out of the ammoniation reactor3And methanol;
c) adding water into the material discharged from the bottom of the methanol removing tower for mixing, and entering a phase separator for extracting the cyclopropane formamide and separating an oil phase and a water phase;
and d) mixing the water phase from the phase separator with NaClO and NaOH aqueous solution, and allowing the mixture to enter a degradation reactor for degradation reaction to generate cyclopropylamine.
The invention provides a continuous production method of cyclopropylamine, the cyclopropylamine obtained in step d) is crude cyclopropylamine, and the production method further comprises the following steps:
and e) separating the material from the degradation reactor through a continuous crude distillation tower and a continuous fine distillation tower to obtain a refined cyclopropylamine product.
Specifically, the material from the degradation reactor is distilled by a continuous crude distillation tower to obtain a cyclopropylamine-containing aqueous solution, and the cyclopropylamine aqueous solution is separated by a continuous fine distillation tower to obtain a pure cyclopropylamine product, namely a cyclopropylamine refined product. The two-stage rectification of the purification of the invention has the following functions: because the equipment of the one-step rectifying tower is too high and complex, the ideal separation effect is difficult to achieve; the two-stage rectification effect is better.
Wherein, the solvent used in the step a) can be selected from dimethylbenzene, methylbenzene, trimethylbenzene and the like. Xylene is preferred.
Wherein, the mol ratio of the methyl chlorobutyrate, the sodium methoxide and the solvent in the step a) is 1: (1-1.5): (0.5-2), the material fluidity and filterability are enhanced.
Wherein the reaction temperature of the cyclization reaction in the step a) is 65-150 ℃, and the reaction pressure is 80-150 Kpa. Preferably, the reaction temperature is 90-110 ℃, and the reaction pressure is 90-110 Kpa.
The cyclization reaction in the step a) is carried out in two-stage reaction distillation kettles (namely a first-stage reaction distillation kettle and a second-stage reaction distillation kettle) which are connected in series, methanol is evaporated while the reaction is carried out, the cyclization reaction is balanced to move towards the direction which is favorable for the generation of methyl cyclopropanecarboxylate, and compared with the method that the two-stage reaction distillation kettles are adopted in the first-stage reaction distillation kettle, the back mixing can be reduced, and the reaction rate and the yield are improved.
Wherein the material discharged from the secondary reaction distillation kettle comprises methyl cyclopropanecarboxylate and solvent.
Wherein the reaction temperature of the ammoniation reaction in the step b) is 35-100 ℃, and the reaction pressure is 0.8-2 MPa. Preferably, the reaction temperature is preferably 70-90 ℃, and the reaction pressure is 1-1.5 Mpa.
Wherein the reaction material in the step b) comprises cyclopropane formamide and NH3And methanol.
According to the production method, ammonia gas and methanol are removed by adopting the ammonia removal tank, the flash tank and the methanol removal tower after the ammoniation reaction is finished. That is to say:
in the step b) of the invention, the ammoniation reaction, namely the reaction product is discharged from the ammoniation reactor and then sequentially enters an ammonia removal tank and a flash tank to remove NH3And part of methanol, and feeding the material from the bottom of the flash tank into a methanol removing tower to further remove the residual methanol.
Wherein, the material that comes out from flash tank bottom contains: cyclopropanecarboxamide, xylene, methanol and sodium chloride.
The function of the ammonia removal tank 4 used in the ammoniation reaction in the step b) of the invention is to stabilize the pressure in the ammoniation reactor 3 and remove part of NH3。
In the step b) of the invention, residual NH is removed by using a flash tank 5 and a methanol removing tower 6 for ammoniation reaction3And residual methanol.
Step c) of the present invention uses a phase separator 7 to separate the solvent and the aqueous solution of cyclopropylcarboxamide. The invention adopts water to extract the cyclopropane formamide, and uses a phase separator to separate a xylene oil phase and a water phase rich in the cyclopropane formamide, thereby removing the solvent (such as xylene).
Wherein the reaction temperature of the degradation reaction in the step d) is-15-30 ℃, and the reaction pressure is 80-150 Kpa. Preferably, the reaction temperature is 5-15 ℃ and the reaction pressure is 110-130 Kpa.
The production method of the invention, methyl chlorobutyrate and NH3The feeding molar ratio of (1) - (3).
According to the production method, water is added in the step c) for extraction, and the feed molar ratio of the cyclopropanecarboxamide to the water is 1 (2-5).
According to the production method, the feeding molar ratio of the cyclopropane carboxamide to the sodium hypochlorite (calculated by available chlorine) is 1 (1.1-2.5).
According to the production method, the feeding molar ratio of the cyclopropane carboxamide to the sodium hydroxide is 1 (2-4).
Production method of the invention, NH3The feed may be ammonia, liquid ammonia or aqueous ammonia, preferably liquid ammonia.
In the production method of the present invention, sodium hypochlorite and sodium hydroxide used in the degradation reaction of cyclopropylamine may be solid or may be their respective aqueous solutions, and preferably their respective aqueous solutions.
The production method of the invention has the advantage that the whole production flow is continuous operation. The trend of the materials in each device is as follows: by utilizing the continuous production system, materials steamed out from the first-stage reaction distillation kettle and the second-stage reaction distillation kettle are mixed with materials discharged from the bottom of the second-stage reaction distillation kettle and then enter the ammoniation reactor, the materials generated from the ammoniation reactor sequentially enter the deammoniation tank, the flash tank, the methanol removal tower and the phase separator, the materials of the phase separator enter the degradation reactor to obtain a cyclopropanamine crude product, and the cyclopropanamine crude product enters the cyclopropanamine continuous crude distillation tower and the cyclopropanamine continuous fine distillation tower to obtain a cyclopropanamine refined product.
The invention has the following beneficial effects: the production system and the production method adopt two stages of reaction distillation kettles, ammoniation reactors, deammoniation tanks, flash tanks, phase separators, degradation reactors, continuous rough distillation towers and rectification tower equipment which are connected in series, can be operated continuously, are beneficial to improving the yield and the production efficiency of the cyclopropylamine, and realize the continuous production in the whole process.
The invention obtains the high-purity cyclopropylamine product, and the total yield of the cyclopropylamine is high. The product quality is high and stable, the labor intensity is low, and the production efficiency of the device is high.
The invention solves the problem of intermittent production of the prior cyclopropylamine; the material fluidity and filterability in the cyclization, ammoniation and ammoniation distillation processes are improved; improves the degradation process of the cyclopropylamide, ensures the achievement of high conversion rate and high yield of the cyclopropylamine, and realizes the continuous production of the cyclopropylamine.
Drawings
FIG. 1 is a schematic view showing the connection of a continuous production system for cyclopropylamine.
Wherein, 1 is a first-stage reaction distillation kettle, 2 is a second-stage reaction distillation kettle, 3 is an ammoniation reactor, 4 is a deammoniation tank, 5 is a flash tank, 6 is a methanol removal tower, 7 is a phase separator, 8 is a degradation reactor, 9 is a continuous crude distillation tower and 10 is a continuous fine distillation tower.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The operations not mentioned in the present invention are all the conventional operations in the art, and the materials mentioned in the present invention are all the conventional materials which can be purchased from the market.
Example 1
The production system for continuously producing the cyclopropylamine comprises the following production devices which are connected in sequence: a first-stage reaction distillation kettle 1, a second-stage reaction distillation kettle 2, a tubular ammoniation reactor 3, a deamination tank 4, a flash tank 5, a methanol removal tower 6, a phase separator 7, a tubular degradation reactor 8, a cyclopropylamine continuous crude distillation tower 9, a cyclopropylamine continuous fine distillation tower 10, equipment connecting pipelines, control instruments and accessories (heat supply, cold supply, safety and the like).
The devices are sequentially connected in sequence, and the material in each device has the following trend (as shown in figure 1): the materials (methanol) steamed out from the first-stage reaction distillation kettle 1 and the second-stage reaction distillation kettle 2 are mixed with the materials (methyl cyclopropanecarboxylate and solvent xylene) discharged from the bottom of the second-stage reaction distillation kettle 2 through a pipeline and then enter the tubular ammonification reactor 3, and the materials (the cyclopropanecarboxamide and the NH) generated by the tubular ammonification reactor 33And methanol) sequentially enter an ammonia removal tank 4, a flash tank 5, a methanol removal tower 6 and a phase separator 7, a material (cyclopropylcarboxamide) of the phase separator 7 enters a tubular degradation reactor 8 to obtain a cyclopropylamine crude product, and the cyclopropylamine crude product enters a cyclopropylamine continuous crude distillation tower 9 and a cyclopropylamine continuous fine distillation tower 10 to obtain a cyclopropylamine refined product.
The method for continuously producing the cyclopropylamine comprises the following steps:
step a) methyl chlorobutyrate, sodium methoxide solid and xylene according to a molar ratio of 1: 1.2: 1, continuously feeding the mixture into a primary reaction distillation kettle, wherein dimethylbenzene is a solvent, methyl chlorobutyrate and sodium methoxide are subjected to cyclization reaction to generate methyl cyclopropanecarboxylate, the reaction temperature is 104 ℃, the pressure is 100kPa, methanol is continuously distilled out in the reaction process, and a product at the bottom of the kettle enters a secondary reaction distillation kettle for further reaction and distillation of the methanol;
step b) methanol distilled from the first-stage reaction distillation kettle and the second-stage reaction distillation kettle, materials (methyl cyclopropanecarboxylate and dimethylbenzene) containing the bottom products of the second-stage reaction distillation kettle and liquid ammonia are mixed and enter a tubular ammoniation reactor, and the methyl cyclopropanecarboxylate and NH3(methyl chlorobutyrate and NH3The feed molar ratio of (1: 2) carrying out an ammoniation reaction in a tubular ammoniation reactor to generate the cyclopropanecarboxamide, wherein the reaction temperature is 80 ℃, the pressure is 1-1.3 MPa, and reaction products sequentially enter an ammonia removal tank and a flash tank to remove NH after coming out of the ammoniation reactor3And part of methanol, and the material coming out of the bottom of the flash tank is removedThe methanol tower further removes the residual methanol;
c) adding water (the feeding molar ratio of the cyclopropanecarboxamide to the water is 1:3) into the material from the bottom of the methanol removing tower, mixing, extracting the cyclopropanecarboxamide in a phase separator, and separating an oil phase and a water phase;
step d) mixing the water phase from the phase separator with NaClO and NaOH aqueous solution (the feeding molar ratio of the cyclopropane formamide and the sodium hypochlorite is 1:2, mixing the cyclopropanecarboxamide and the sodium hydroxide according to a feeding molar ratio of 1:3), and allowing the mixture to enter a tubular degradation reactor to perform degradation reaction at 10-13 ℃ and a pressure of 120Kpa to generate cyclopropylamine;
and e) separating the material from the degradation reactor by using a cyclopropylamine continuous crude distillation tower to obtain a cyclopropylamine-containing aqueous solution, and rectifying the cyclopropylamine solution distilled from the top of the cyclopropylamine continuous crude distillation tower in a cyclopropylamine continuous fine distillation tower to obtain a cyclopropylamine product with the purity of 99.95%, wherein the total yield is 93%.
Example 2
This embodiment is the same as embodiment 1 except that: during the cyclization reaction, 30% sodium methoxide methanol solution is adopted as sodium methoxide feed. The purity of the cyclopropylamine product is 99.95%, and the total yield is 92%.
Example 3
This embodiment is the same as embodiment 1 except that: the reactor for the degradation reaction adopts a kettle type reactor, and the reaction temperature is controlled at 0-13 ℃. The purity of the cyclopropylamine product is 99.95%, and the total yield is 91%.
Example 4
This embodiment is the same as embodiment 1 except that: methyl chlorobutyrate, sodium methoxide solid and xylene in a molar ratio of 1: 1.5: 2. the purity of the cyclopropylamine product is 99.95%, and the total yield is 91%.
The solvent used in step a) of the invention can be replaced by toluene or trimethylbenzene, and the corresponding effect can also be realized.
Comparative example
The intermittent production process of the cyclopropylamine is as follows: in a cyclization reaction kettle, methyl chlorobutyrate, 30% sodium methoxide methanol solution and xylene are mixed according to a molar ratio of 1: 1.2: 1, adding sodium methoxide and methyl chlorobutyrate to react in a solvent to generate methyl cyclopropanecarboxylate, controlling the temperature of a reaction kettle to be about 140 ℃, cooling after full reaction, and then sending the reacted materials containing sodium chloride, methyl cyclopropanecarboxylate, dimethylbenzene and methanol to a high-pressure ammoniation reaction kettle; adding liquid ammonia into a high-pressure ammoniation reaction kettle for ammoniation reaction, carrying out the ammoniation reaction under the condition of heat preservation, controlling the temperature to be 70-85 ℃ and the pressure to be 0.5-1.5 MPa, cooling to discharge excessive ammonia after the reaction is finished, transferring the material into a methanol xylene distillation kettle, adding water after the material in the kettle is semi-solid, and conveying a water layer to a cyclopropane carboxamide degradation reaction kettle; adding alkali liquor and sodium hypochlorite solution into a cyclopropanecarboxamide degradation kettle for degradation reaction, keeping the reaction temperature at-10-0 ℃, and transferring the material to a pre-distillation kettle after full reaction; the distillation operation of the pre-distillation kettle of the crude distillation is finished until the kettle temperature is 115 ℃, and the residual liquid containing sodium carbonate and sodium chloride is discharged to a geosyncline; the raw material of the cyclopropylamine crude distillation kettle is from the distillation product obtained in the previous step, the cyclopropylamine crude distillation kettle is added with caustic soda flakes to remove ammonia, and then the pre-fraction is steamed to a degradation normal-fraction aqueous solution storage tank for 2 hours, and then the normal-fraction is steamed to the crude distillation normal-fraction aqueous solution storage tank, and the steaming is finished at the top temperature of 80 ℃; the raw material of the cyclopropylamine rectifying still comes from the crude distilled normal water liquid storage tank in the previous step, caustic soda flakes are added to remove ammonia, and the refined cyclopropylamine product is obtained after distillation is carried out until the internal temperature is about 80 ℃.
The whole production flow is intermittently operated, the purity of the finally obtained product is 90.9 percent, and the yield is about 79 percent.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (6)
1. A cyclopropylamine continuous production method is characterized in that a cyclopropylamine continuous production device is used for production, and the cyclopropylamine continuous production device comprises the following production devices which are sequentially connected: one-level reaction stills (1), second grade reaction stills (2), ammoniation reactor (3), deammoniation jar (4), flash tank (5), methanol removal tower (6), phase separator (7), degradation reactor (8), crude distillation tower (9) and smart distillation column (10), its characterized in that includes following step:
step a), continuously feeding methyl chlorobutyrate, sodium methoxide and a solvent into a primary reaction distillation kettle, carrying out cyclization reaction on the methyl chlorobutyrate and the sodium methoxide to generate methyl cyclopropanecarboxylate, continuously distilling out methanol in the reaction process, feeding a kettle bottom product of the primary reaction distillation kettle into a secondary reaction distillation kettle for further reaction and distilling the methanol;
step b) methanol distilled from the first-stage reaction distillation kettle and the second-stage reaction distillation kettle, and materials and NH discharged from the second-stage reaction distillation kettle3Mixing the mixture with methyl cyclopropanecarboxylate and NH in an ammoniation reactor3Performing ammoniation reaction to generate the cyclopropanecarboxamide, wherein the reaction temperature is 70-90 ℃, the reaction pressure is 1-1.5 Mpa, and the reaction materials sequentially enter an ammonia removal tank, a flash tank and a methanol removal tower to remove NH after coming out of the ammoniation reactor3And methanol;
c) adding water into the material discharged from the bottom of the methanol removing tower for mixing, and entering a phase separator for extracting the cyclopropane formamide and separating an oil phase and a water phase;
mixing the water phase from the phase separator in the step d) with NaClO and NaOH aqueous solution, and allowing the mixture to enter a degradation reactor for degradation reaction to generate a crude product of cyclopropylamine, wherein the reaction temperature is 5-15 ℃, and the reaction pressure is 110-130 Kpa;
and e) separating the material from the degradation reactor through a crude distillation tower and a fine distillation tower to obtain a refined cyclopropylamine product.
2. The continuous production method of cyclopropylamine according to claim 1, wherein the solvent is xylene, toluene or trimethylbenzene.
3. The continuous production method of cyclopropylamine according to claim 1, wherein the molar ratio of methyl chlorobutyrate, sodium methoxide and solvent in step a) is 1: (1-1.5): (0.5-2).
4. The continuous production method of cyclopropylamine according to claim 1, wherein the cyclization reaction in step a) is carried out at a reaction temperature of 65 to 150 ℃ and a reaction pressure of 80 to 150 Kpa.
5. The continuous process for producing cyclopropylamine of claim 1, wherein methyl chlorobutyrate and NH are used3The feeding molar ratio of (1) to (3);
adding water for extraction, wherein the feed molar ratio of the cyclopropanecarboxamide to the water is 1 (2-5);
the feeding molar ratio of the cyclopropanecarboxamide to the sodium hypochlorite is 1 (1.1-2.5);
the feeding molar ratio of the cyclopropane formamide to the sodium hydroxide is 1 (2-4).
6. The continuous production method of cyclopropylamine of claim 1, wherein the reaction product of step b) is discharged from the ammoniation reactor and then enters into the ammonia removal tank and the flash tank to remove NH3And part of methanol, and feeding the material from the bottom of the flash tank into a methanol removing tower to further remove the residual methanol.
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Denomination of invention: A continuous production system and method for cyclopropylamine Effective date of registration: 20230427 Granted publication date: 20210625 Pledgee: Taizhou Linhai sub branch of Bank of Communications Co.,Ltd. Pledgor: Zhejiang Shaxing Technology Co.,Ltd. Registration number: Y2023330000807 |