Acrylate preparation method

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

Inactive Publication Date: 2015-03-18
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

[0024] 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.

[0025] Preparation of Mo-based metal complex catalysts. Take 0.004molMoCl 3 and 0.006mol 1,3-bis(diphenylphosphine)propane were added to the Schlenk reaction bottle, and then 0.02molg sodium amalgam was added, the reaction bottle was connected to the Schlenk device, and the air in the bottle was purged with high-purity argon. Replacement to ensure the anhydrous and oxygen-free environment in the reaction bottle and Schlenk device. After three replacements, use a vacuum pump to pump the reaction bottle to a negative pressure state, and move 70ml of tetr...

example 2

[0028] Preparation of Mo-based metal complex catalysts. Take 0.003molMoCl 3 Add 0.007mol1,3-bis(diphenylphosphine)propane into the Schlenk reaction bottle, then add 0.018molg sodium amalgam, connect the reaction bottle to the Schlenk device, and use high-purity argon to replace the air in the bottle , to ensure the anhydrous and oxygen-free environment in the reaction bottle and the Schlenk device. After three replacements, use a vacuum pump to pump the reaction bottle to a negative pressure state, and move 100ml of tetrahydrofuran that has undergone anhydrous and oxygen-free treatment into the reaction bottle with a needle. , under the protection of high-purity argon, stirred at 10°C for 150min, and distilled off the solvent from the obtained solution at 70°C under reduced pressure to obtain a Mo-based metal complex catalyst.

[0029] CO 2The reaction process of synthesizing acrylate with ethylene is carried out in the Schlenk device. Under anhydrous and oxygen-free conditi...

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 Mo-based metal complex catalysts. Take 0.004molMoCl 3 Add 0.014mol 1,3-bis(diphenylphosphine)propane into the Schlenk reaction bottle, then add 0.01mol sodium amalgam, connect the reaction bottle to the Schlenk device, and use high-purity argon to replace the air in the bottle , to ensure the anhydrous and oxygen-free environment in the reaction bottle and the Schlenk device. After three replacements, the reaction bottle was pumped to a negative pressure state with a vacuum pump, and 90ml of tetrahydrofuran treated with anhydrous ...

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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 under the action of a methylation reagent by using CO2 and ethylene as raw materials, acetonitrile as a solvent and a metal Mo complex as a catalyst, wherein the mole ratio of the raw material ethylene to carbon dioxide is (1 to 1)-(1 to 5), preferably (1 to 2)-(1 to 4); the gas flow rate is 1-20ml / min, preferably 3-15ml / min; the reaction temperature is minus 5-50 DEG C, preferably 0-40 DEG C; the reaction pressure is 0.01-0.5MPa, preferably 0.05-0.4MPa. 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 Applications(China)
IPC IPC(8): C07C69/54C07C67/00
CPCC07C67/00C07C69/54
Inventor 孙潇磊张志智尹泽群刘全杰张喜文
Owner CHINA PETROLEUM & CHEM CORP
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