Method for synthesizing acrylic acid

An acrylic acid and complex technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylates, etc., can solve the problems of expensive catalysts, difficult to control catalyst loss, harsh reaction conditions, etc., and achieve catalytic activity and reaction. High selectivity, ease of scale-up and industrial application, mild reaction conditions

Inactive Publication Date: 2019-04-05
XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the reaction conditions are mild, but the catalyst is relatively expensive. The most important thing is that the stability of the catalyst is poor. The main reason is that the catalyst is a homogeneous catalyst, and the loss of the catalyst is not easy to control.
[0006] Zhao Yonglu and others from Xinjiang Zhongtai Chemical used palladium catalysts supported by inorganic substances to obtain the results that the conversion rate of acetylene can reach more than 99%, and the yield of acrylic acid can reach more than 97%. The complicated process of separation and recycling
[0007] In a word, the main problem of the catalyst of acetylene carbonylation to acrylic acid (ester) is that either the reaction conditions are harsh, or the catalyst is a homogeneous catalyst, the catalyst is easy to lose, or the process is complicated

Method used

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  • Method for synthesizing acrylic acid

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Experimental program
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Effect test

Embodiment 1

[0023] Preparation of acid functionalized ionic liquid palladium phosphine ligand complex catalyst supported by NaY molecular sieve:

[0024] a. Add 10g NaY molecular sieve and 25ml methyl imidazole to a 250ml Erlenmeyer flask in turn, stir at room temperature for 8h, then add 75ml of decane bromide into the Erlenmeyer flask, stir at a temperature of 50°C for 12h, filter , washed 3 times with 30ml absolute ethanol, dried to obtain 8g white solid powder;

[0025] b. Add 8 g of white solid powder obtained in step a, 30 ml of organic solvent ethyl acetate into a 100 ml conical flask in turn, add 2 g of organic acid p-toluenesulfonic acid, stir for 12 hours at a temperature of 50 ° C, filter, and use 30 Washed 3 times with absolute ethanol, dried to obtain 9g white solid powder;

[0026] c. Add 9g of white solid powder obtained in step b and 30ml of distilled water to a 100ml Erlenmeyer flask in turn, and add 2ml of 0.28mol / L H 2 PdCl 4 Solution, after stirring continuously for...

Embodiment 2

[0030] Preparation of acid functionalized ionic liquid palladium phosphine ligand complex catalyst supported by NaY molecular sieve:

[0031] a. Add 15g NaY molecular sieve and 50ml methyl imidazole to a 250ml Erlenmeyer flask in turn, stir at room temperature for 12h, then add 120ml of decane bromide into the Erlenmeyer flask, stir at a temperature of 80°C for 6h, filter , washed 3 times with 60ml absolute ethanol, dried to obtain 11g white solid powder;

[0032] b. Add 11g of white solid powder obtained in step a, 30ml of organic solvent acetone to a 100ml Erlenmeyer flask successively, add 4g of organic acid trifluoromethanesulfonic acid, stir at a temperature of 80°C for 6 hours, filter, and use 60ml of Washed with water and ethanol for 3 times, dried to obtain 12g white solid powder;

[0033] c. Add 12g of white solid powder obtained in step b and 30ml of distilled water to a 100ml Erlenmeyer flask, and add 4.8ml of 0.28mol / L H 2 PdCl 4 After stirring continuously for ...

Embodiment 3

[0037] Preparation of acid functionalized ionic liquid palladium phosphine ligand complex catalyst supported by NaY molecular sieve:

[0038] a. Add 12g NaY molecular sieve and 35ml methyl imidazole to a 250ml conical flask in turn, stir at room temperature for 10 hours, then add 100ml bromodecane to the conical flask, and stir for another 8 hours at a temperature of 60°C , filtered, washed 3 times with 45ml of absolute ethanol, and dried to obtain 9.5g of white solid powder;

[0039] b. Add 9.5g of white solid powder obtained in step a and 30ml of organic solvent tetrahydrofuran into a 100ml conical flask in turn, add 3g of organic acid p-toluenesulfonic acid, stir for another 10 hours at a temperature of 70°C, filter, and use 40ml Wash with absolute ethanol for 3 times, and dry to obtain about 10.5g of white solid powder;

[0040] c. Add 10.5g of white solid powder obtained in step b and 30ml of distilled water to a 100ml Erlenmeyer flask in turn, and add 3.6ml of 0.28mol / L...

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Abstract

The invention relates to a method for synthesizing acrylic acid. The method includes leading methylimidazole and decyl bromide into NaY molecular sieve cages and synthesizing ionic liquid in an in-situ manner; further leading organic acid into the ionic liquid and preparing NaY molecular sieve supported acid functional ionic liquid; sequentially leading Pd2+, N and P ligands into molecular sieve supercages and forming palladium coordination compounds in an in-situ manner to obtain NaY molecular sieve supported acid functional ionic liquid palladium phosphine ligand complex compound catalysts;catalyzing carbonylation of acetylene under the effects of the catalysts to synthesize the acrylic acid. The method has the advantages that the stability of the catalysts can be greatly enhanced by the aid of the method, the conversion rate of the acetylene can reach 99% at least, and the yield of the acrylic acid can reach 98% at least, and still can be 98% after the catalysts are reused by 10 times.

Description

technical field [0001] The invention relates to a method for synthesizing acrylic acid. Background technique [0002] As an important chemical raw material, acetylene can synthesize a series of important compounds. At present, the largest use is to synthesize vinyl chloride, which is then polymerized into polyvinyl chloride (PVC). However, due to the current oversupply of PVC production capacity, almost all PVC manufacturers are in a situation of meager profit or loss. Therefore, it is necessary to develop a production process that can replace PVC, provide a new development route for PVC manufacturers, and at the same time enable acetylene manufacturers to achieve better development, and more importantly, it can stabilize a large number of PVC and PVC Ethylene-related industries, such as acetylene, calcium carbide, coal chemical industry and other industries. [0003] A review of the relevant industrial production process of acetylene and relevant literature shows that ac...

Claims

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Application Information

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IPC IPC(8): C07C57/04C07C51/145B01J31/24B01J31/02B01J29/08
CPCC07C51/145B01J29/084B01J31/0284B01J31/2495B01J2231/321B01J2531/824B01J2531/0213B01J35/19C07C57/04Y02P20/54
Inventor 李弘毅马昱博王磊
Owner XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST
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