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Application of plasma modified phosphotungstic heteropolyacid in synthesis of adiponitrile from adipic acid

A plasma and heteropolyacid technology, applied in the field of adiponitrile synthesis, can solve the problems of reactor corrosion, affect normal production, increase production cost, etc. Effect

Active Publication Date: 2020-04-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst faces a series of problems: firstly, a large amount of phosphoric acid and phosphoric acid ester will cause certain corrosion to the reactor and affect normal production; secondly, this type of liquid catalyst is easily soluble in the reaction system, causing catalyst loss and increasing Production cost; finally, phosphoric acid, etc. will generate polymers in the reaction, affecting heat transfer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0031] h 4 (PW 11 VO 40 ) preparation: first weigh 3.80g disodium hydrogen phosphate and dissolve it in 20mL deionized water, then weigh 36.3g sodium tungstate and dissolve it in 80mL deionized water, and finally weigh 1.22g sodium metavanadate and dissolve it in 10mL with a concentration of 1.0 mol / L sodium carbonate solution. Add the above-mentioned disodium hydrogen phosphate solution dropwise to the sodium tungstate aqueous solution, add the sodium metavanadate solution after the dropwise addition, and then use about 2 mL of sulfuric acid aqueous solution with a mass concentration of 50% to adjust the pH value of the solution to about 2.5, at 90 °C under constant stirring and reflux for 2 h. After the reaction, the solution was cooled to room temperature, and then poured into a 500 mL separatory funnel. First add 30 mL of ether, then add a small amount of 50% sulfuric acid aqueous solution in multiple times, shake evenly for extraction. A total of 25 mL of sulfuric ac...

Embodiment 2

[0033] h 6 (PW 9 V 3 o 40 ) preparation: Weigh 60g of sodium tungstate and dissolve it in 75mL of deionized water, then add 1.8-2.0mL of phosphoric acid solution (85wt.%) dropwise under continuous stirring, and finally add about 10mL of glacial acetic acid, while vigorously stirring, there will be A white precipitate formed. Continue to stir for 1 hour, filter and dry after the completion of the reaction to obtain a white powder PW 9 . 8.2 g of sodium acetate was dissolved in 100 mL of deionized water in a 250 mL beaker, and an aqueous solution of acetic acid (35%) was added dropwise until the pH of the solution was 4.8. To the above solution was added 3.949 g of sodium metavanadate and 20 g of unheated crude product PW 9 , the solution was stirred at 25°C for 48 hours or at 90°C for 2 hours. After the solution is cooled, pour it into a 500mL separatory funnel, then add 35mL of ether, and add a small amount of sulfuric acid aqueous solution with a mass concentration of ...

Embodiment 3

[0035] h 7 (P 2 W 17 VO 62 ) Synthesis of heteropolyacid: Weigh 28.04g sodium tungstate and 1.56g disodium hydrogen phosphate and dissolve them in 100mL deionized water, add dropwise an aqueous solution of sulfuric acid with a mass concentration of 50%, when the pH value of the solution reaches 3-4, Then add 0.7898g of sodium metavanadate, and react for 8h under the condition of heating and reflux, and cool to room temperature after the reaction. The cooled solution was transferred into a 500mL separatory funnel, 30mL of ether was added, and a small amount of sulfuric acid aqueous solution (5mL) with a mass concentration of 50% was added in portions, fully oscillated, and separated into three layers after standing. The red oily substance in the lower layer was heteropolyacid etherate. Carry out vacuum drying to obtain the red powder, put the above red powder into a plasma treatment device, and discharge it at 20W for 30min under hydrogen atmosphere to obtain catalyst C.

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Abstract

The invention provides application of a plasma modified phosphotungstic heteropolyacid catalyst in synthesis of adiponitrile from adipic acid. The plasma modified phosphotungstic heteropolyacid catalyst is used for catalyzing adipic acid to be ammoniated and dehydrated to synthesize adiponitrile. The synthesis of the phosphotungstic heteropolyacid catalyst adopts an acidification-diethyl ether extraction method, that is, heteroatom oxyacid and ligand atom oxyacid or ligand atom oxide are uniformly mixed according to a certain proportion, and after long-time heating reflux, heteropolyacid is obtained through acidification treatment. The heteropolyacid is subjected to a reaction with diethyl ether under an acidic condition to form an oily substance, diethyl ether is volatilized to obtain solid heteropolyacid, and plasma treatment is carried out on the solid heteropolyacid to obtain the plasma-modified solid heteropolyacid. Phosphorus-containing anions generated by the phosphotungstic heteropolyacid catalyst in a solution are used as catalysts, so that the acidity in the solution is reduced, the chemical reaction environment of adiponitrile synthesis is changed, the conversion rate and the selectivity of a chemical reaction are improved, and the generation of carbon deposit is reduced.

Description

technical field [0001] The invention belongs to the technical field of adiponitrile synthesis, and in particular relates to the application of a plasma-modified phosphotungstic heteropolyacid in the synthesis of adiponitrile by reacting adipic acid and ammonia. Background technique [0002] As an important chemical raw material, adiponitrile can react with hydrogen to form hexamethylenediamine, and hexamethylenediamine and adipic acid react under strict material ratio to form nylon 66 salt. Therefore, adiponitrile, as an important intermediate in the synthesis of nylon 66, is the most important and most valuable industrial use of adiponitrile. [0003] At present, the methods for synthesizing adiponitrile mainly include electrolytic dimerization of acrylonitrile (AN), butadiene (BD) and catalytic amination of adipic acid (ADA). Among them, the adipic acid ammonification method is the first industrialized method for the synthesis of adiponitrile. At present, the method is di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J35/10C07C255/04C07C253/22
CPCB01J27/188C07C253/22B01J35/61C07C255/04
Inventor 黄家辉张少华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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