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CN-121988245-A - Production device and production method of monoethylamine

CN121988245ACN 121988245 ACN121988245 ACN 121988245ACN-121988245-A

Abstract

The application discloses a production device and a production method of monoethylamine, which adopt a cyclic operation process of raw material preheating-hydrogenation reaction-gradient pressure swing condensation-expansion deep cooling-multi-extraction rectification-byproduct recycling, so that acetonitrile is hydrogenated to generate a hydrogenation product containing monoethylamine, the product is refined to obtain the monoethylamine product, and meanwhile, the byproduct diethyl amine and triethylamine are recycled, so that the raw material conversion rate and the monoethylamine process yield are effectively improved, and meanwhile, unreacted hydrogen is recycled, so that the raw material conversion rate is further improved, the operation is convenient, and the method is suitable for industrial large-scale production.

Inventors

  • DING HUI
  • HUANG SHENGJUN
  • LI PEIDONG
  • ZHANG DAZHI

Assignees

  • 中国科学院大连化学物理研究所

Dates

Publication Date
20260508
Application Date
20241106

Claims (10)

  1. 1. A production device of monoethylamine, which is characterized by comprising a first preheater and a second preheater which are connected with a reactor; The reactor is also sequentially connected with a cooler, a first liquid separating tank, a circulating compressor, a deep cooler, a heat exchanger, a second liquid separating tank and a product tower; The bottom of the first liquid separating tank is connected with the product tower; the heat exchanger is also connected with the first preheater; The top of the second liquid separation tank is also connected with the heat exchanger through an expander; The bottom of the product tower is connected with the second preheater; the heat exchanger and the product column are provided with discharge ports, respectively.
  2. 2. The apparatus for producing monoethylamine according to claim 1, wherein a sub heater is further provided before the inlet of the reactor.
  3. 3. The apparatus for producing monoethylamine according to claim 1, wherein the first liquid separation tank is a water-cooled liquid separation tank, and the second liquid separation tank is a cryogenic liquid separation tank.
  4. 4. A process for the production of monoethylamine using the apparatus of any one of claims 1 to 3, comprising the steps of: S1, introducing hydrogen into a first preheater for preheating; acetonitrile is led into a second preheater for preheating; then mixing the preheated hydrogen and acetonitrile to form mixed raw material gas; S2, sending the mixed feed gas into a reactor for hydrogenation reaction to obtain a hydrogenation reaction product, sending the hydrogenation reaction product into a cooler for cooling, and then sending the cooled hydrogenation reaction product into a first liquid separation tank for gas-liquid separation to obtain a first gas phase and a first liquid phase; The first gas phase is sent to the circulating compressor for pressurization treatment, then is sent to the deep cooler and the heat exchanger in sequence for cooling, and finally is sent to a second liquid separating tank for gas-liquid separation, so as to obtain a second gas phase and a second liquid phase; s3, sending the second gas phase into an expander for adiabatic expansion, sending the second gas phase into a heat exchanger for recycling cold energy, and then discharging part of the second gas phase as a byproduct, and sending the rest of the second gas phase to the first preheater for recycling; s4, feeding the first liquid phase and the second liquid phase into a product tower, and extracting through a fractional condensation rectification side line; non-condensable gas and liquid ammonia are obtained at the top of the product tower, and monoethylamine is obtained at the middle part of the product tower; And obtaining a mixture of diethylamine and triethylamine at the bottom of the product tower, discharging part of the mixture as a byproduct, and sending the rest of the mixture to the second preheater for recycling.
  5. 5. The method of claim 4, wherein the heating temperature of the first preheater and the second preheater is 40-200 ℃.
  6. 6. The method according to claim 4, wherein the reaction temperature of the reactor is 110-200 ℃ and the operating pressure is 3-30 bar (a).
  7. 7. The method of claim 4, wherein the cooler is operated at a temperature of 20-120 ℃; The cryogenic temperature of the refrigerator is-35 to-10 ℃.
  8. 8. The method of claim 4, wherein the operating pressure of the first knock out pot is 3-30 bar (a); Preferably, the operating pressure of the second liquid separation tank is 20-100 bar (A).
  9. 9. The method according to claim 4, wherein the outlet pressure of the recycle compressor is 20-100 bar (a); preferably, the outlet temperature of a hot flow of the heat exchanger is-60 to-35 ℃; Preferably, the outlet pressure of the expander is 3-30 bar (A).
  10. 10. The method according to claim 4, wherein the product column has a column top temperature of-40 to 0 ℃, a column top pressure of 3 to 10bar (A), a theoretical plate number of 20 to 80, and a reflux ratio of 10 to 100.

Description

Production device and production method of monoethylamine Technical Field The application relates to a production device and a production method of monoethylamine, and belongs to the field of chemical industry. Background The ethylamine compound is an important organic chemical raw material and is widely applied to synthesis of solvents, pesticides, pharmacy, fine chemical industry, high-energy fuel, surfactants and intermediates. At present, the synthesis process of ethylamine compounds is mainly an ethanol ammonification method, but the product of the process is limited by reaction balance, so that the product is a mixture of monoethylamine, diethyl amine and triethylamine, the yield of a single target product is not high and is difficult to promote, and therefore, the process is not suitable for industrial scale production, and a preparation method of monoethylamine which has high pertinence, can realize high conversion rate of raw materials, is simple and convenient and is suitable for industrial scale production is needed to be discovered, but the corresponding process research has not been reported yet, and further research is needed. Disclosure of Invention According to one aspect of the present application, there is provided a production apparatus for monoethylamine, comprising a first preheater and a second preheater connected to a reactor; The reactor is also sequentially connected with a cooler, a first liquid separating tank, a circulating compressor, a deep cooler, a heat exchanger, a second liquid separating tank and a product tower; The bottom of the first liquid separating tank is connected with the product tower; the heat exchanger is also connected with the first preheater; The top of the second liquid separation tank is also connected with the heat exchanger through an expander; The bottom of the product tower is connected with the second preheater; the heat exchanger and the product column are provided with discharge ports, respectively. Optionally, a secondary heater is further arranged in front of the inlet of the reactor. Optionally, the first liquid separating tank is a water-cooled liquid separating tank, and the second liquid separating tank is a cryogenic liquid separating tank. According to another aspect of the present application, there is also provided a method for producing monoethylamine using the above apparatus, comprising the steps of: S1, introducing hydrogen into a first preheater for preheating; acetonitrile is led into a second preheater for preheating; then mixing the preheated hydrogen and acetonitrile to form mixed raw material gas; S2, sending the mixed feed gas into a reactor for hydrogenation reaction to obtain a hydrogenation reaction product, sending the hydrogenation reaction product into a cooler for cooling, and then sending the cooled hydrogenation reaction product into a first liquid separation tank for gas-liquid separation to obtain a first gas phase and a first liquid phase; the first gas phase consists of a hydrogen/ammonia mixture and a small amount of ethylamine, and the first liquid phase consists of mixed ethylamine; The first gas phase is sent to the circulating compressor for pressurization treatment, then is sent to the deep cooler and the heat exchanger in sequence for cooling, and finally is sent to a second liquid separating tank for gas-liquid separation, so as to obtain a second gas phase and a second liquid phase; The second gas phase is deaminated circulating hydrogen, and the second liquid phase is a mixture of ethylamine and ammonia; s3, sending the second gas phase into an expander for adiabatic expansion, sending the second gas phase into a heat exchanger for recycling cold energy, and then discharging part of the second gas phase as a byproduct, and sending the rest of the second gas phase to the first preheater for recycling; s4, feeding the first liquid phase and the second liquid phase into a product tower, and extracting through a fractional condensation rectification side line; non-condensable gas and liquid ammonia are obtained at the top of the product tower, and monoethylamine is obtained at the middle part of the product tower; The non-condensable gas is discharged as waste gas, and the liquid ammonia is discharged as a byproduct; And obtaining a mixture of diethylamine and triethylamine at the bottom of the product tower, discharging part of the mixture as a byproduct, and sending the rest of the mixture to the second preheater for recycling. Optionally, the heating temperature of the first preheater and the second preheater is 40-200 ℃. Optionally, the reaction temperature of the reactor is 110-200 ℃ and the operating pressure is 3-30 bar (A). Optionally, the operation temperature of the cooler is 20-120 ℃; the cryogenic temperature of the refrigerator is-35 to-10 ℃; it should be noted that the chiller may be split into 2-3 heat exchangers in series according to the type of refrigerant. Optionally, the operating pressure