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A kind of synthetic method of acrylate

A technology of acrylate and synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low propylene conversion rate and methacrylate yield, etc. The effect of improving the reactivity

Active Publication Date: 2016-08-17
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Propylene conversion rate and methacrylate yield are low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Anhydrous and oxygen-free treatment of solvents. The water removal process of acetonitrile and tetrahydrofuran adopts P 2 o 5 and anhydrous Na 2 SO 4 Dry overnight, carry out the deoxygenation process in a distillation flask in the presence of Na or benzophenone, evaporate the solvent after acetonitrile is refluxed at 85°C for 3 hours, and evaporate the solvent after tetrahydrofuran is refluxed at 75°C for 3 hours.

[0024] Preparation of Ni-based metal complex catalysts. Take 1.31gNi(cod) 2 Dissolve in 40ml of tetrahydrofuran, add 1.91g of 1,3-bis(diphenylphosphine)propane to the solution, and then add 0.35g of succinic acid, stir the resulting solution at 5°C for 40min, and filter with suction to obtain the Ni-based metal complex Catalyst, kept in the glove box for future use.

[0025] CO 2 The reaction process of synthesizing acrylate with ethylene is carried out in an autoclave, first add 10g of anhydrous Na to the autoclave 2 CO 3 And seal the autoclave, r...

example 2

[0027] Anhydrous and oxygen-free treatment of solvents. The water removal process of acetonitrile and tetrahydrofuran adopts P 2 o 5 and anhydrous Na 2 SO 4 Dry overnight, deoxygenate in the presence of Na or benzophenone in a distillation flask, acetonitrile is refluxed at 85°C for 3 hours and the solvent is distilled off for later use, tetrahydrofuran is refluxed at 75°C for 3 hours and the solvent is evaporated for later use.

[0028] Preparation of Ni-based metal complex catalysts. Take 1.15gNi(cod) 2 Dissolve it in 50ml of tetrahydrofuran, add 5.04g of 1,3-bis(diphenylphosphine)propane to the solution, and then add 0.27g of succinic acid, stir the resulting solution at 10°C for 110min, and filter with suction to obtain the Ni-based metal complex Catalysts were stored in the glove box for future use.

[0029] CO 2 The reaction process of synthesizing acrylate with ethylene is carried out in an autoclave, first add 20g of anhydrous Na to the autoclave 2 CO 3And the...

example 3

[0031] Anhydrous and oxygen-free treatment of solvents. The water removal process of acetonitrile and tetrahydrofuran adopts P 2 o 5 and anhydrous Na 2 SO 4 Dry overnight, carry out the deoxygenation process in a distillation flask in the presence of Na or benzophenone, evaporate the solvent after acetonitrile is refluxed at 85°C for 3 hours, and evaporate the solvent after tetrahydrofuran is refluxed at 75°C for 3 hours.

[0032] Preparation of Ni-based metal complex catalysts. Take 1.30gNi(cod) 2 Dissolve it in 40ml of tetrahydrofuran, add 7.21g of 1,3-bis(diphenylphosphine)propane to the solution, and then add 0.35g of succinic acid, stir the resulting solution at 0°C for 70min, and filter with suction to obtain the Ni-based metal complex Catalyst, kept in the glove box for future use.

[0033] CO 2 The reaction process of synthesizing acrylate with ethylene is carried out in an autoclave, first add 12g of anhydrous Na to the autoclave 2 CO 3 And the autoclave is s...

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PUM

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Abstract

The invention discloses an acrylate synthesis method. The method is characterized by directly synthesizing acrylate by adopting batch reaction, using CO2 and ethylene as raw materials, acetonitrile as a solvent, a metal Ni complex as a catalyst and anhydrous sodium carbonate as a promoter, and adding a methylation reagent to continuously react for 10-24 hours after reacting for 15-30 hours, wherein the mole ratio of ethylene to carbon dioxide is (1 to 1)-(1 to 5), preferably (1 to 2)-(1 to 4); the reaction temperature is 40-130 DEG C, preferably 50-120 DEG C; the reaction pressure is 0.5-6.0MPa, preferably 1.0-5.5MPa. In the method, acrylate is directly synthesized under the action of the methylation reagent by using CO2 and ethylene as the raw materials. The method has the advantages of low reaction temperature, high product yield, and the like.

Description

technical field [0001] The present invention relates to a kind of synthetic method of acrylic acid ester, relate in particular to a kind of 2 A method of directly synthesizing acrylate with ethylene as raw material. Background technique [0002] With the increasing dependence of modern society on petrochemical resources, increasing CO 2 The emission problem is not only an environmental problem, but has risen to the level of international relations and human survival and development. CO 2 The greenhouse effect caused by the rapid increase will seriously threaten the survival of human beings. Global energy shortages and CO 2 The increasingly serious environmental problems caused by it force people to find ways to solve these problems, so as to devote themselves to CO 2 processing utilization. The most direct CO 2 The treatment method is how to consume more CO 2 , to achieve CO 2 recycling to fundamentally solve CO 2 question. CO 2 The chemical utilization is to ach...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/54C07C67/00
CPCC07C67/00C07C69/54
Inventor 孙潇磊张志智尹泽群刘全杰宋喜军张喜文
Owner CHINA PETROLEUM & CHEM CORP
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