Method for producing adiponitrile with adipic acid liquid-phase method

A technology of adipic acid liquid and adiponitrile, applied in chemical instruments and methods, purification/separation of carboxylic acid nitrile, organic chemistry, etc., can solve problems that have not yet appeared

Active Publication Date: 2016-11-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is worth noting that the solid phosphoric acid catalyst has only been used in the adipic acid gas phase process, and has not yet appeared in the adipic acid liquid phase process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Dry 10g of diatomaceous earth in an oven at 120°C for 2 hours; then soak it in 120g of phosphoric acid solution with a concentration of 75% by mass, and add 6g of aluminum sulfate solution with a concentration of 20% by mass to form a mixed solution; stir the mixed solution After 12 hours, let it stand for 12 hours; centrifuge the mixed solution, and place the obtained precipitate in an oven at 120°C to dry for 12 hours; place the dried precipitate in a tubular roaster, and continuously feed N 2 , and calcined at 400° C. for 2 hours to finally form a solid phosphoric acid catalyst; press the calcined solid phosphoric acid catalyst into tablets, and screen to obtain 20-40 mesh particles.

[0071] The application of solid phosphoric acid catalyst in adipic acid liquid phase method is as follows:

[0072] In the aforementioned adipic acid liquid-phase process, the input amount of adipic acid is 73g, the input amount of adiponitrile is 146g, the solid phosphoric acid input ...

Embodiment 2

[0074] Change the concentration of phosphoric acid in the preparation process of solid phosphoric acid in Example 1 to 75% by mass percentage, the amount of phosphoric acid solution added is 100g, the amount of copper sulfate solution with a concentration of 20% by mass percentage is 5g, and the drying temperature is 100°C, stirring for 6h After standing still for 6 hours, the calcination temperature was changed to 600° C., and other conditions remained unchanged to obtain a solid phosphoric acid catalyst.

[0075] In the aforesaid adipic acid liquid-phase process, the amount of solid phosphoric acid input accounts for 1.0% of the total input amount of reactants, the stirring speed is 1000r / min, and other process conditions are the same as in Example 1. It was found that after 60 minutes of reaction, the dehydration rate reached 69.8%.

Embodiment 3

[0077] Change the phosphoric acid concentration in the preparation process of embodiment 1 solid phosphoric acid to 65% of the mass percentage concentration, the add-on of phosphoric acid solution is 150g, the add-on of aluminum sulfate solution is 7.5g, the roasting temperature is changed into 400 ℃, drying temperature is 140 °C, and other conditions remain unchanged, a solid phosphoric acid catalyst is obtained.

[0078] In the aforementioned adipic acid liquid-phase process, the input amount of adipic acid is 200g, the input amount of adiponitrile is 400g, the solid phosphoric acid input amount accounts for 2.1% of the total input amount of the reactant, and the ammonia flow rate is 400L / h, the stirring speed is 2000r / min, and the reaction temperature is 280°C. It was found that after 60 minutes of reaction, the dehydration rate reached 91.6%.

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PUM

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Abstract

The invention discloses a method for producing adiponitrile with an adipic acid liquid-phase method. A solid phosphoric acid catalyst is adopted, adipic acid and a diluent are added into a reaction still, heating and raw material stirring are conducted during reaction, ammonia gas is supplied after temperature reaches a certain value, and the product is generated after reaction is conducted for a while. A novel environment-friendly adiponitrile synthesis method is adopted. By the adoption of the solid phosphoric acid catalyst, the defects of traditional catalysts are overcome, and catalysis effect is improved.

Description

technical field [0001] The invention relates to a technology for producing adiponitrile by liquid-phase ammoniation of adipic acid. A green solid phosphoric acid catalyst is used in the production. Background technique [0002] Adiponitrile is an important raw material for nylon 66, and there is a large market demand in China. Among them, the adipic acid catalytic ammonification method is an important industrial process in the production of adiponitrile. Catalytic ammoniation of adipic acid is a process in which adipic acid and ammonia react to form crude adiponitrile under the action of a dehydration catalyst, and the finished product is obtained after rectification. According to the different physical states of adipic acid, the process is divided into adipic acid liquid phase method and adipic acid gas phase method. Among them, the reaction temperature of the liquid phase method is generally about 280°C, and the reaction temperature of the gas phase method is 350°C-420°C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/32C07C255/04B01J27/182B01J27/185
Inventor 史君张晓琳陈丰秋范立耸程党国詹晓力冯赛平王洪星曹志涛张英杰董大清赵晶
Owner PETROCHINA CO LTD
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