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Preparation method for metal complex catalyst used for synthesis of acrylic acid

A metal complex and catalyst technology, which is applied in the field of metal complex catalyst preparation, can solve problems such as low propylene conversion rate and low methacrylate yield, and achieve the effects of being beneficial to activation and improving reaction activity

Active Publication Date: 2014-05-14
CHINA PETROLEUM & CHEM CORP +1
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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

[0019] 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 in the presence of benzophenone, reflux at 85°C for 2 hours, then distill off the solvent for later use; tetrahydrofuran in the presence of Na and benzophenone , After reflux at 75°C for 2h, the solvent was distilled off for later use.

[0020] Preparation of metal Ni complex catalysts. Take 1.05gNi(cod) 2 Dissolve in 40mL tetrahydrofuran, add 3.05g 1,3-bis(diphenylphosphine)propane to the solution, and then add 0.30g succinic acid, stir the resulting solution at 5°C for 45min, and filter with suction to obtain the Ni-based metal complex Catalyst, kept in the glove box for future use.

[0021] CO 2 The reaction process of synthesizing acrylic acid with ethylene is carried out in an autoclave. Firstly, the autoclav...

example 2

[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, deoxygenate in the presence of Na or benzophenone in a distillation flask, acetonitrile in the presence of benzophenone, reflux at 85°C for 2 hours, and distill off the solvent for later use; tetrahydrofuran in the presence of Na and benzophenone , After reflux at 75°C for 2h, the solvent was distilled off for later use.

[0024] Preparation of Ni-based metal complex catalysts. Take 1.05gNi(cod) 2 Dissolve in 50mL tetrahydrofuran, add 4.58g 1,3-bis(diphenylphosphine)propane to the solution, and then add 0.25g 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.

[0025] CO 2 The reaction process of synthesizing acrylic acid with ethylene is carried out in an autoclave. Firstly, the aut...

example 3

[0027] Anhydrous and oxygen-free treatment of solvents. The dehydration 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 in the presence of benzophenone, reflux at 85°C for 2 hours, and distill off the solvent for later use; tetrahydrofuran in the presence of Na and benzophenone , After reflux at 75°C for 2h, the solvent was distilled off for later use.

[0028]Preparation of Ni-based metal complex catalysts. Take 1.30gNi(cod) 2 Dissolve in 40mL tetrahydrofuran, add 7.21g 1,3-bis(diphenylphosphine)propane to the solution, and then add 0.35g succinic acid, stir the resulting solution at 10°C for 110min, and filter with suction to obtain the Ni-based metal complex Catalyst, kept in the glove box for future use.

[0029] CO 2 The reaction process of synthesizing acrylic acid with ethylene is carried out in an autoclave. First, the autocl...

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Abstract

The invention discloses a preparation method for a metal complex catalyst used for synthesis of acrylic acid. The method comprises the following steps: dissolving bis(1,5-cyclooctadiene)nickel [Ni(cod)2]; then adding ligand and organic acid, carrying out stirring at a temperature of -10 to 30 DEG C for 10 to 150 min, preferably, at a temperature of -5 to 20 DEG C for 20 to 120 min; and finally, carrying out filtering and drying so as to prepare the metal complex catalyst used for synthesis of acrylic acid. The catalyst prepared by using the method has the advantages of low reaction temperature, high yield of acrylic acid and the like when used in direct synthesis of acrylic acid from CO2 and ethene.

Description

technical field [0001] The invention relates to a preparation method of a metal complex catalyst for synthesizing acrylic acid, in particular to a method for CO 2 A method for preparing a metal complex catalyst for synthesizing acrylic acid with ethylene. 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 questio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24C07C57/04C07C51/15
Inventor 孙潇磊张志智尹泽群刘全杰
Owner CHINA PETROLEUM & CHEM CORP
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