Method of synthesizing methyl acetate through acetylene carbonylation

A technology for the synthesis of methyl acrylate, which is applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, organic compound/hydride/coordination complex catalysts, etc., can solve problems affecting industrial applications and homogeneous catalysts Difficult to recycle and other issues

Active Publication Date: 2016-07-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the homogeneous catalyst is difficult to separate from the produ

Method used

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  • Method of synthesizing methyl acetate through acetylene carbonylation
  • Method of synthesizing methyl acetate through acetylene carbonylation
  • Method of synthesizing methyl acetate through acetylene carbonylation

Examples

Experimental program
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Embodiment 1

[0020] N-PPOL preparation method: In a liquid nitrogen bath and a nitrogen atmosphere, add 45ml of tetrahydrofuran, 0.12mol of n-butyllithium, 0.1mol of o-bromopyridine, 0.135mol of ZnCl 2 , 45ml pyridine, 90ml tetrahydrofuran, and react at room temperature for 14h. Pour out the liquid in the bottle under nitrogen protection, then add 60ml of pyridine, 180ml of tetrahydrofuran, and 0.12mol of PCl3 solution (dissolved in 60ml of pyridine and 60ml of tetrahydrofuran) successively under the condition of a liquid nitrogen bath, and then react at room temperature for 26h (named as reaction Liquid 1). In a liquid nitrogen bath and a nitrogen atmosphere, add 0.22mol (5.4g) of magnesium chips, 35ml of tetrahydrofuran, and 36.6g (0.2mol) of p-bromostyrene to another 1L three-necked round-bottomed flask with a magnetic stirring bar. (named as reaction solution 2). After the reaction solution 1 was filtered, it was added to the reaction solution 2 in a liquid nitrogen bath and a nitro...

Embodiment 2

[0023] Tetrahydrofuran was used instead of acetone as the solvent, and other conditions were the same as in Example 1.

Embodiment 3

[0025] Adopt normal hexane to replace acetone as solvent, other conditions are the same as embodiment 1.

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Abstract

The invention provides a method of synthesizing methyl acetate through acetylene carbonylation.The method includes: using acetylene, methanol and carbon monoxide as reaction raw materials; under conditions with reaction temperature of 30-80 DEG C and initial pressure of 1,2-6.5 MPa, adopting a palladium-based catalyst immobilized by organic ligand polymer to catalyze acetylene carbonylation to synthesize methyl acetate.2-pyridyldiphenylphosphine (2-PyPPh2) is adopted as an organic ligand and grafted with vinyl to prepare vinyl2-pyridyldiphenylphosphine, cross-linking polymerization is performed under certain conditions to form solid organic ligand polymer (N-PPOL), and the organic ligand polymer is complexed and immobilized with palladium acetate to prepare the palladium-based catalyst immobilized by the organic ligand polymer.Methyl acetate is synthesized through acetylene carbonylation in one step and has high activity, high selectivity and high easiness in separation and recycling.

Description

technical field [0001] The invention relates to a method for synthesizing methyl acrylate by carbonylation of acetylene, in particular to a method using acetylene, methanol and carbon monoxide as reaction raw materials, under the conditions of a reaction temperature of 30-80°C and an initial pressure of 1.2-6.5MPa. A palladium-based catalyst supported by an organic ligand polymer can catalyze the carbonylation of acetylene to prepare methyl acrylate. Background technique [0002] Methyl acrylate is the simplest aliphatic unsaturated ester. Since its molecular structure has unsaturated double bonds, it can form many different types of polymers through self-polymerization or copolymerization. These polymers have the characteristics of good transparency, light stability and water absorption, and are widely used in the fields of coatings, textiles, adhesives, papermaking additives, glazing agents, leather additives, detergents, and superabsorbent materials. At present, propylen...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/38B01J31/24
CPCY02P20/50
Inventor 丁云杰陈兴坤朱何俊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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