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4-aminobutyronitrile preparation method and device adopting pyrrolidone liquid phase method

A technology of pyrrolidone liquid and aminobutyronitrile, which is applied in the field of preparation of aminobutyronitrile, can solve the problems of less by-products, high reaction conversion rate, and low temperature of liquid phase method, so as to improve product quality, high product conversion rate, and reaction simple effect

Pending Publication Date: 2021-06-18
PINGDINGSHAN PUEN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But take pyrrolidone as raw material to prepare the patent of aminocapronitrile less, take pyrrolidone as raw material to prepare the method for 2-aminocapronitrile at present according to the reaction state of pyrrolidone and can be divided into gas-phase method and two kinds of liquid-phase methods, wherein gas-phase method temperature is high, The reaction consumes a lot of energy, and there are many reaction by-products; the liquid phase method has low temperature, mild reaction conditions, less by-products, and high reaction conversion

Method used

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  • 4-aminobutyronitrile preparation method and device adopting pyrrolidone liquid phase method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] like figure 1 Shown, a kind of preparation device that utilizes pyrrolidone liquid phase method to prepare 4-aminobutyronitrile, comprises ammonia gas preprocessor 1, reactor 2, ammonia water separator 3, condenser 4 and gas-liquid separator 5; The new ammonia gas of the processor 1 and the recovered ammonia gas enter the reactor 2 in series, the gas outlet of the reactor 2 is connected with the inlet of the ammonia water separator 3, and the gas outlet of the ammonia water separator 3 is connected with the inlet of the condenser 4 The gas outlet of the condenser 4 is connected with the gas inlet of the gas-liquid separator 5, and the gas outlet of the gas-liquid separator 5 is connected with the gas inlet of the reactor 1; Shuikou, unreacted ammonia gas and new ammonia gas enter the reaction kettle 2 in series to continue the reaction.

[0034] Wherein: the ammonia water separator 3 is equipped with packing, and the circulating water in the condenser 4 is a circulatin...

Embodiment 2

[0039] Heat 100g of pyrrolidone, 1000g of succinonitrile, and 1g of boron phosphate to 100°C in a reaction kettle connected with an ammonia water separator, preheat the ammonia gas after the ammonia gas pre-treatment to 100°C, and start the stirring speed at 1000RPM, When the temperature reaches 200°C, ammonia gas is introduced, and the molar ratio of ammonia gas to pyrrolidone is 10:1 during the reaction, and the reaction lasts for 2 hours. After the reaction was completed, the upper tower was distilled under reduced pressure, the temperature of the bottom of the tower was 130°C, the temperature of the top of the tower was 110°C, and the negative pressure was -0.095MPA to obtain 4-aminobutyronitrile with a purity of 99.7%.

[0040] After product metering and analysis, the selectivity of pyrrolidone in this example was 98.50%, and the conversion rate was 65.00%.

[0041] The technical indicators of ammonia gas before and after activated carbon adsorption are shown in the table...

Embodiment 3

[0046] Heat 100g of pyrrolidone, 800g of succinonitrile, and 2g of boron phosphate in a reaction kettle with an ammonia water separator to 110°C, preheat the ammonia gas after ammonia pretreatment to 110°C, and start the stirring speed at 1200RPM. When the temperature reaches 230°C, ammonia gas is introduced, and the molar ratio of ammonia gas to pyrrolidone is 20:1 during the reaction, and the reaction lasts for 2 hours. After the reaction was completed, the upper tower was distilled under reduced pressure, the temperature of the bottom of the tower was 150°C, the temperature of the top of the tower was 125°C, and the negative pressure was -0.085MPA to obtain 4-aminobutyronitrile with a purity of 99.6%.

[0047] After product measurement and analysis, the selectivity of pyrrolidone in this example was 98.80%, and the conversion rate was 68.50%.

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Abstract

The invention discloses a 4-aminobutyronitrile preparation method and device adopting a pyrrolidone liquid phase method. The preparation method comprises the following steps: mixing pyrrolidone and an organic solvent, and preheating at the preheating temperature of 90-110 DEG C; purifying and preheating ammonia gas, with the preheating temperature being 90-110 DEG C; fully mixing the pyrrolidone, the organic solvent and a catalyst, heating to a certain temperature, and introducing the ammonia gas into a reaction kettle for reaction; and after the reaction is finished, carrying out reduced pressure distillation on the reaction product to obtain the product 4-aminobutyronitrile. The preparation device comprises an ammonia gas pretreatment device, a reaction kettle, an ammonia water separator, a condenser and a gas-liquid separator, wherein a gas outlet of the reaction kettle is communicated with a gas inlet of the ammonia water separator, a gas outlet of the ammonia water separator is communicated with a gas inlet of the condenser, a gas outlet of the condenser is communicated with a gas inlet of the gas-liquid separator, a gas outlet of the gas-liquid separator is communicated with a gas inlet of the reaction kettle, and a water outlet is formed in the gas-liquid separator. The method and the device are low in energy consumption, easy in reaction, high in conversion rate and stable in product quality.

Description

technical field [0001] The invention belongs to the technical field of preparation of aminobutyronitrile, and in particular relates to a method and a device for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method. Background technique [0002] Aminobutyronitrile is an important chemical intermediate, an important intermediate in organic synthesis and pharmaceutical synthesis. At present, the preparation of aminobutyronitrile is mainly through the reaction of n-propionaldehyde and excess cyanide followed by vacuum distillation, such as patent number CN201911196336.9. But take pyrrolidone as raw material to prepare the patent of aminocapronitrile less, take pyrrolidone as raw material to prepare the method for 2-aminocapronitrile at present according to the reaction state of pyrrolidone and can be divided into gas-phase method and two kinds of liquid-phase methods, wherein gas-phase method temperature is high, The reaction consumes a lot of energy and...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C253/00C07C255/24C01C1/02
CPCC07C253/20C07C253/00C01C1/024C07C255/24Y02P20/52
Inventor 陈聚良屈建海陈亚春朱子强刘水侠李云鹏刘荣鸽张乐堂王允从刘浩勇张朝领司松凡
Owner PINGDINGSHAN PUEN TECH CO LTD
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