CN115920788A - Amination reaction system - Google Patents
Amination reaction system Download PDFInfo
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- CN115920788A CN115920788A CN202211658177.1A CN202211658177A CN115920788A CN 115920788 A CN115920788 A CN 115920788A CN 202211658177 A CN202211658177 A CN 202211658177A CN 115920788 A CN115920788 A CN 115920788A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/584—Recycling of catalysts
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Abstract
The invention relates to an amination reaction system which comprises a raw material tank, an inert gas buffer tank, a liquid ammonia tank, an ammonia buffer tank, a raw material microwave preheater, an inert gas preheater, an ammonia gas preheater, a microwave heater, a fluidized bed reactor, a condenser, a gas-liquid separator, a product tank, an inert gas separation tower, an inert gas refining tower, a pressure swing adsorption separation tower, an ammonia gas refining tower and a liquid tank. The system has the characteristics of good heat transfer performance, uniform and easily-controlled temperature in the bed layer of the reactor, convenience for continuous regeneration and circulation of the catalyst, high utilization rate of the catalyst and ammonia, less ammonia gas amount and the like. The process system breaks through the existing process route; wherein, the ammonia which is not fully reacted is recovered, thereby more efficiently utilizing the ammonia and reducing the using amount of the ammonia; meanwhile, the inert gas is also separated, recycled and reused, thereby further reducing the energy consumption.
Description
Technical Field
The invention relates to the technical field of organic chemical industry, in particular to an amination reaction system.
Background
According to patent CN201711061104.3, a method for preparing cyclohexylamine by cyclohexanol aminolysis is introduced, wherein a catalyst is formed by hydrotalcite or hydrotalcite-like composite transition metal simple substance active components.
Patent CN201810001682.6 describes a catalyst for the aminolysis reaction between aldehydes or ketones and ammonia in a hydrogen atmosphere.
Patent CN202110164835.0 describes a process for preparing adiponitrile by amination and dehydration of adipic acid.
Patent CN202010374890.8 describes a catalyst composition for ester amination dehydration reaction and a preparation method of L-menthane carboxamide.
Patent CN201910775834.2 introduces a catalyst for preparing 6-aminocapronitrile by caprolactam amination and dehydration reaction.
Patent No. cn201310355337.X describes a process for the ammonolysis of aromatic chlorides to aniline compounds, using a catalyst which is a 13X molecular sieve treated by cuprous ion exchange.
Products prepared by related amination reactions (such as adiponitrile and 6-aminocapronitrile which are intermediates for synthesizing hexamethylene diamine) are important intermediates, so that the amination reaction system provided by the invention has the characteristics of good heat transfer performance, uniform and easily-controlled temperature in a reactor bed, convenience for continuous regeneration and circulation of a catalyst, high catalyst utilization rate, high ammonia utilization rate, small ammonia amount and the like, and is particularly important.
Disclosure of Invention
The invention aims to provide an amination reaction system, which solves the problems of large ammonia source utilization amount, low utilization rate and high energy consumption of a conventional amination reaction system.
In order to solve the technical problem, the invention adopts the following technical scheme:
the invention provides an amination reaction system, which comprises a raw material tank, a raw material microwave preheater, an inert gas tank, an inert gas buffer tank, an inert gas preheater, a liquid ammonia tank, an ammonia buffer tank, an ammonia preheater, a mixed gas buffer tank, a microwave heater, a reactor, a condenser, a gas-liquid separator, a product tank, an inert gas separation tower, an inert gas refining tower, a pressure swing adsorption separation tower, an ammonia refining tower and a liquid tank, wherein the raw material tank is connected with the inert gas buffer tank;
the raw material tank, the liquid ammonia tank and the inert gas tank are respectively communicated with the mixed gas buffer tank through pipelines; wherein the conveying pipelines of the raw material tank, the liquid ammonia tank and the inert gas tank are respectively preheated by a raw material microwave preheater, an ammonia gas preheater and an inert gas preheater;
the mixed gas buffer tank is connected with a feed inlet of the reactor through a pipeline, a product of the reactor is conveyed to the condenser through a pipeline, the condenser is connected with the gas-liquid separator through a pipeline, and a microwave heater is arranged on the pipeline between the mixed gas buffer tank and the reactor;
a liquid phase outlet of the gas-liquid separator is connected with the product tank, and a gas phase outlet of the gas-liquid separator is connected with the inert gas separation tower through a pipeline;
the top of the inert gas separation tower is connected with the inert gas refining tower through a pipeline, and a refined product of the inert gas refining tower flows back to the inert gas buffer tank; the top of the inert gas separation tower is connected with the pressure swing adsorption separation tower through a pipeline;
the top of the pressure swing adsorption separation tower is connected with the ammonia gas refining tower through a pipeline, wherein the refined ammonia gas flows back to the ammonia gas buffer tank; the top of the pressure swing adsorption separation tower is connected with a liquid tank through a pipeline.
Further, the raw material reactant in the raw material tank is one or more of compounds such as alcohols, aldehydes, ketones, acids, esters, amides, halogenated hydrocarbons and the like.
Still further, the reactor is a fluidized bed reactor or a fixed bed reactor.
Still further, the reactor is a fluidized bed reactor and is provided with a catalyst regeneration device.
And further, the inert gas tank is connected with the inert gas buffer tank through a pipeline, and then is connected with the mixed gas buffer tank through the inert gas buffer tank.
And further, the liquid ammonia tank is connected with the ammonia buffer tank through a pipeline, and then is connected with the mixed gas buffer tank through the ammonia buffer tank.
Still further, the method also comprises the following application steps:
s1, mixing preheated ammonia gas and inert gas, mixing with the preheated raw materials, and feeding the mixture into a reactor;
s2, condensing the gas-liquid mixture after reaction by a condenser, then feeding the gas-liquid mixture into a gas-liquid separator, allowing the product, raw materials which may not be completely reacted and a side reaction product to flow into a liquid tank, and allowing ammonia gas, inert gas and a small amount of other gas substances to flow into an inert gas separation tower;
s3, the inert gas separation tower operates under a certain pressure, the gas-phase inert gas flows from the top of the tower to the inert gas refining tower for refining and then is reused, and the liquid-phase ammonia and the possible residual byproducts, products and raw materials flow into the pressure swing adsorption separation tower together;
and S4, the pressure swing adsorption tower is mainly used for separating ammonia, the ammonia flows to an ammonia refining tower from the top of the tower, the ammonia is refined and reused, and residual byproducts, products, raw materials and the like after pressure relief at the bottom of the tower flow to a liquid tank from the bottom of the tower.
Compared with the prior art, the invention has the beneficial technical effects that: the process system breaks through the existing process route; wherein, the ammonia which is not fully reacted is recovered, thereby more efficiently utilizing the ammonia and reducing the using amount of the ammonia; meanwhile, the inert gas is also separated, recycled and reused, thereby further reducing the energy consumption.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is a schematic diagram of an amination reaction system according to the invention.
Description of reference numerals: 1. a raw material tank, a is a raw material pipeline, and 2 is a raw material microwave preheater; 3 is an inert gas tank, b is an inert gas pipeline, 4 is an inert gas buffer tank, and 5 is an inert gas preheater; 6 is a liquid ammonia tank, c is an ammonia pipeline, 7 is an ammonia buffer tank, and 8 is an ammonia preheater; 9 is a mixed gas buffer tank, d is a mixed gas pipeline; 10 is a microwave heater, 11 is a reactor, and e is a material pipeline after reaction; 12 is a condenser, f is a condensed material pipeline; 13 is a gas-liquid separator, g is a product pipeline, and 14 is a product tank; h is a gas phase pipeline, 15 is an inert gas separation tower, i is an inert gas pipeline, 16 is an inert gas refining tower, and j is refined inert gas; k is a liquefied ammonia line, 17 is a pressure swing adsorption separation column, m is a liquid line in which one or more of by-products, raw materials, and ammonia may remain, 18 is a liquid tank, n is separated gaseous ammonia, 19 is an ammonia gas purification column, and o is purified ammonia gas.
Detailed Description
The embodiment discloses an amination reaction system, which comprises a raw material tank 1, a raw material microwave preheater 2, an inert gas tank 3, an inert gas buffer tank 4, an inert gas preheater 5, a liquid ammonia tank 6, an ammonia buffer tank 7, an ammonia preheater 8, a mixed gas buffer tank 9, a microwave heater 10, a reactor 11, a condenser 12, a gas-liquid separator 13, a product tank 14, an inert gas separation tower 15, an inert gas refining tower 16, a pressure swing adsorption separation tower 17, an ammonia refining tower 19 and a liquid tank 18;
the raw material tank 1, the liquid ammonia tank 6 and the inert gas tank 3 are respectively communicated with the mixed gas buffer tank 9 through pipelines; wherein the conveying pipelines of the raw material tank 1, the liquid ammonia tank 6 and the inert gas tank 3 are respectively preheated by a raw material microwave preheater 2, an ammonia gas preheater 8 and an inert gas preheater 5;
the mixed gas buffer tank 9 is connected with a feed inlet of a reactor 11 through a pipeline, a product of the reactor 11 is conveyed to the condenser 12 through a pipeline, the condenser 12 is connected with the gas-liquid separator 13 through a pipeline, and a microwave heater 10 is arranged on the pipeline between the mixed gas buffer tank 9 and the reactor 11;
a liquid phase outlet of the gas-liquid separator 13 is connected with the product tank 14, and a gas phase outlet of the gas-liquid separator 13 is connected with the inert gas separation tower 15 through a pipeline;
the top of the inert gas separation tower 15 is connected with the inert gas refining tower 16 through a pipeline, and a refined product of the inert gas refining tower 16 flows back to the inert gas buffer tank 4; the top of the inert gas separation tower 15 is connected with the pressure swing adsorption separation tower 17 through a pipeline;
the top of the pressure swing adsorption separation tower 17 is connected with the ammonia refining tower 19 through a pipeline, wherein refined ammonia flows back to the ammonia buffer tank 7; the bottom of the pressure swing adsorption separation tower 17 is connected with a liquid tank 18 through a pipeline; the pressure swing adsorption separation tower 17 is a pressure swing adsorption tower and is mainly used for separating ammonia, the ammonia flows to an ammonia refining tower from the top of the tower and is reused after refining, and residual byproducts, products, raw materials and the like after pressure relief at the bottom of the tower flow to a liquid tank from the bottom of the tower. Trace reactants such as byproducts, products, water, raw materials and the like can be carried in the ammonia gas, the ammonia gas (the ammonia gas can carry trace water) flows out of the adsorption tower from the top of the tower after pressure swing adsorption, liquid such as water flows to the liquid tank, and the liquid in the liquid tank can be transferred to the product tank after being accumulated to a certain degree. According to different systems, the product in the product tank can be further refined to obtain a pure product.
In this embodiment, the raw material reactant in the raw material tank 1 is one or more of compounds such as alcohols, aldehydes, ketones, acids, esters, amides, halogenated hydrocarbons, and the like.
Wherein the reactor 11 is a fluidized bed reactor or a fixed bed reactor.
Wherein the reactor 11 is a fluidized bed reactor and is provided with a catalyst regeneration device.
The inert gas tank 3 is connected with the inert gas buffer tank 4 through a pipeline, and is connected with the mixed gas buffer tank 9 through the inert gas buffer tank 4.
Wherein the liquid ammonia tank 6 is connected with the ammonia buffer tank 7 through a pipeline, and then is connected with the mixed gas buffer tank 9 through the ammonia buffer tank 7.
Example 1
As shown in fig. 1, an amination reaction system comprises: 1. a raw material tank, a is a raw material pipeline, and 2 is a raw material microwave preheater; 3 is an inert gas tank, b is an inert gas pipeline, 4 is an inert gas buffer tank, and 5 is an inert gas preheater; 6 is a liquid ammonia tank, c is an ammonia pipeline, 7 is an ammonia buffer tank, and 8 is an ammonia preheater; 9 is a mixed gas buffer tank, d is a mixed gas pipeline; 10 is a microwave heater, 11 is a reactor, and e is a material pipeline after reaction; 12 is a condenser, f is a condensed material pipeline; 13 is a gas-liquid separator, g is a product pipeline, and 14 is a product tank; h is a gas phase pipeline, 15 is an inert gas separation tower, i is an inert gas pipeline, 16 is an inert gas refining tower, and j is refined inert gas; k is a liquefied ammonia line, 17 is a pressure swing adsorption separation column, m is a liquid line in which one or more of by-products, raw materials, and ammonia may remain, 18 is a liquid tank, n is separated gaseous ammonia, 19 is an ammonia gas purification column, and o is purified ammonia gas.
The amination and dehydration operation of caprolactam by utilizing the amination reaction system comprises the following steps:
(1) Mixing preheated ammonia gas and nitrogen gas, mixing the mixture with preheated caprolactam, and feeding the mixture into a fixed bed reactor, wherein the molar ratio of the ammonia gas to the caprolactam is 6, the molar ratio of the nitrogen gas to the caprolactam is 3, the reaction temperature is 350 ℃, and the reaction pressure is slight positive pressure;
(2) Condensing the reacted gas-liquid mixture through a condenser, then feeding the condensed gas-liquid mixture into a gas-liquid separator, allowing 6-aminocapronitrile, caprolactam, water and other side reaction products to flow into a liquid tank, and allowing ammonia gas, nitrogen gas and a small amount of other gas substances to flow into a nitrogen gas separation tower;
(3) After the nitrogen separation tower is pressurized to a certain degree, gas-phase nitrogen flows to a nitrogen refining tower from the top of the tower and is refined and reused, and liquid-phase ammonia, residual 6-aminocapronitrile, caprolactam, water and other side reaction products flow to a pressure swing adsorption separation tower together;
(4) The pressure swing adsorption tower separates out gaseous ammonia, the ammonia flows to the ammonia refining tower from the top of the tower, the ammonia is reused after being refined, and the 6-aminocapronitrile, caprolactam, water and other side reaction products and the like flow to the liquid tank from the bottom of the tower after the pressure is released at the bottom of the tower.
Caprolactam conversion 97.1% and 6-aminocapronitrile selectivity 98.2%.
Example 2
The amination and dehydration operation of caprolactam by utilizing the amination reaction system comprises the following steps:
(1) Mixing preheated ammonia gas and nitrogen gas, mixing the mixture with preheated caprolactam, and feeding the mixture into a fluidized bed reactor, wherein the molar ratio of the ammonia gas to the caprolactam is 5, the molar ratio of the nitrogen gas to the caprolactam is 2, the reaction temperature is 310 ℃, and the reaction pressure is slight positive pressure;
(2) Condensing the reacted gas-liquid mixture through a condenser, then feeding the condensed gas-liquid mixture into a gas-liquid separator, allowing 6-aminocapronitrile, caprolactam, water and other side reaction products to flow into a liquid tank, and allowing ammonia gas, nitrogen gas and a small amount of other gas substances to flow into a nitrogen gas separation tower;
(3) After the nitrogen separation tower is pressurized to a certain degree, gas-phase nitrogen flows to a nitrogen refining tower from the top of the tower and is refined for reuse, and liquid-phase ammonia, residual 6-aminocapronitrile, caprolactam, water and other side reaction products flow to the pressure swing adsorption separation tower together;
(4) The pressure swing adsorption tower separates out gaseous ammonia, the ammonia flows to the ammonia refining tower from the top of the tower, the ammonia is reused after being refined, and the 6-aminocapronitrile, caprolactam, water and other side reaction products and the like flow to the liquid tank from the bottom of the tower after the pressure is released at the bottom of the tower.
Caprolactam conversion 98.4% and 6-aminocapronitrile selectivity 99.1%.
Example 3
The amination reaction system is used for preparing acetonitrile by acetic acid amination and dehydration, and the operation process is as follows:
(1) Mixing preheated ammonia gas and nitrogen gas, mixing the mixture with preheated acetic acid, and feeding the mixture into a fluidized bed reactor, wherein the molar ratio of the ammonia gas to the acetic acid is 1.2, the molar ratio of the nitrogen gas to the acetic acid is 1, the reaction temperature is 340 ℃, and the reaction pressure is micro-positive pressure;
(2) Condensing the reacted gas-liquid mixture through a condenser, then feeding the condensed gas-liquid mixture into a gas-liquid separator, allowing acetonitrile, water and other side reaction products to flow into a liquid tank, and allowing ammonia gas, nitrogen gas and a small amount of other gas substances to flow into a nitrogen gas separation tower;
(3) After the nitrogen separation tower is pressurized to a certain degree, gas-phase nitrogen flows to a nitrogen refining tower from the top of the tower and is refined for reuse, and liquid-phase ammonia, residual acetonitrile, water and other side reaction products flow to the pressure swing adsorption separation tower together;
(4) The pressure swing adsorption tower separates out gaseous ammonia, the ammonia flows to the ammonia refining tower from the top of the tower, the ammonia is reused after being refined, and acetonitrile, water and other side reaction products and the like flow to the liquid tank from the bottom of the tower after pressure relief.
The acetic acid conversion rate is 100%, and the acetonitrile selectivity is 99.5%.
Example 4
The amination reaction system is used for preparing acetonitrile by acetic acid amination and dehydration, and the operation process is as follows:
(1) Mixing preheated ammonia gas and nitrogen gas, mixing the mixture with preheated acetic acid, and feeding the mixture into a fixed bed reactor, wherein the molar ratio of the ammonia gas to the acetic acid is 1.5, the molar ratio of the nitrogen gas to the acetic acid is 1.2, the reaction temperature is 360 ℃, and the reaction pressure is micro-positive pressure;
(2) Condensing the reacted gas-liquid mixture through a condenser, then feeding the condensed gas-liquid mixture into a gas-liquid separator, allowing acetonitrile, water and other side reaction products to flow into a liquid tank, and allowing ammonia gas, nitrogen gas and a small amount of other gas substances to flow into a nitrogen gas separation tower;
(3) After the nitrogen separation tower is pressurized to a certain degree, gas-phase nitrogen flows to a nitrogen refining tower from the top of the tower and is refined for reuse, and liquid-phase ammonia, residual acetonitrile, water and other side reaction products flow to the pressure swing adsorption separation tower together;
(4) The pressure swing adsorption tower separates out gaseous ammonia, the ammonia flows to the ammonia refining tower from the top of the tower, the ammonia is reused after being refined, and acetonitrile, water and other side reaction products and the like flow to the liquid tank from the bottom of the tower after pressure relief.
The acetic acid conversion rate is 100%, and the acetonitrile selectivity is 99.2%.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used merely for convenience in describing the present invention, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The above embodiments are only for describing the preferred mode of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (7)
1. An amination reaction system, characterized by: the device comprises a raw material tank, a raw material microwave preheater, an inert gas tank, an inert gas buffer tank, an inert gas preheater, a liquid ammonia tank, an ammonia buffer tank, an ammonia preheater, a mixed gas buffer tank, a microwave heater, a reactor, a condenser, a gas-liquid separator, a product tank, an inert gas separation tower, an inert gas refining tower, a pressure swing adsorption separation tower, an ammonia refining tower and a liquid tank;
the raw material tank, the liquid ammonia tank and the inert gas tank are respectively communicated with the mixed gas buffer tank through pipelines; preheating is carried out on the conveying pipelines of the raw material tank, the liquid ammonia tank and the inert gas tank through a raw material microwave preheater, an ammonia gas preheater and an inert gas preheater respectively;
the mixed gas buffer tank is connected with a feed inlet of the reactor through a pipeline, a product of the reactor is conveyed to the condenser through a pipeline, the condenser is connected with the gas-liquid separator through a pipeline, and a microwave heater is arranged on the pipeline between the mixed gas buffer tank and the reactor;
a liquid phase outlet of the gas-liquid separator is connected with the product tank, and a gas phase outlet of the gas-liquid separator is connected with the inert gas separation tower through a pipeline;
the top of the inert gas separation tower is connected with the inert gas refining tower through a pipeline, and a refined product of the inert gas refining tower flows back to the inert gas buffer tank; the top of the inert gas separation tower is connected with the pressure swing adsorption separation tower through a pipeline;
the top of the pressure swing adsorption separation tower is connected with the ammonia gas refining tower through a pipeline, wherein the refined ammonia gas flows back to the ammonia gas buffer tank; the bottom of the pressure swing adsorption separation tower is connected with a liquid tank through a pipeline.
2. The amination reaction system of claim 1, characterized in that: the raw material reactant in the raw material tank is one or more of compounds such as alcohols, aldehydes, ketones, acids, esters, amides, halogenated hydrocarbons and the like.
3. The amination reaction system according to claim 1, characterized in that: the reactor is a fluidized bed reactor or a fixed bed reactor.
4. The amination reaction system according to claim 3, characterized in that: the reactor is a fluidized bed reactor and is provided with a catalyst regeneration device.
5. The amination reaction system according to claim 1, characterized in that: the inert gas tank is connected with the inert gas buffer tank through a pipeline, and then is connected with the mixed gas buffer tank through the inert gas buffer tank.
6. The amination reaction system of claim 1, characterized in that: the liquid ammonia tank is connected with the ammonia buffer tank through a pipeline, and then is connected with the mixed gas buffer tank through the ammonia buffer tank.
7. The amination reaction system of claim 1, characterized in that: the method comprises the following application steps:
s1, mixing preheated ammonia gas and inert gas, mixing with the preheated raw materials, and feeding the mixture into a reactor;
s2, condensing the gas-liquid mixture after reaction by a condenser, then feeding the gas-liquid mixture into a gas-liquid separator, allowing the product, raw materials which may not be completely reacted and a side reaction product to flow into a liquid tank, and allowing ammonia gas, inert gas and a small amount of other gas substances to flow into an inert gas separation tower;
s3, the inert gas separation tower operates under a certain pressure, the gas-phase inert gas flows from the top of the tower to the inert gas refining tower for refining and then is reused, and the liquid-phase ammonia and the possible residual byproducts, products and raw materials flow into the pressure swing adsorption separation tower together;
and S4, the pressure swing adsorption tower is mainly used for separating ammonia, the ammonia flows to an ammonia refining tower from the top of the tower, the ammonia is refined and reused, and the residual byproducts, products, raw materials and the like after pressure relief at the bottom of the tower flow to a liquid tank from the bottom of the tower.
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