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Phase-transfer catalyst quaternary ammonium salt and preparation method thereof

A phase-transfer catalyst and quaternary ammonium salt technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the synthesis process of heteropolyacid quaternary ammonium salt catalysts Complexity, catalyst residue, long reaction time, etc.

Inactive Publication Date: 2012-09-19
JIANGSU TETRA NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the practical application of the catalytic oxidation process in the invention patent with the publication number CN101143919, the catalytic oxidation selectivity is low, the yield of alicyclic epoxy compounds, especially the epoxy resin ERL-4221, is only about 50%, and the catalyst is easy to be deposited in the product. remaining problems in the laboratory research phase only
Patent No. CN200810010953.0 describes the heteropolyacid quaternary ammonium salt catalyst synthesis process is more complicated, the reaction time is long, in the catalytic oxidation reaction need to use a co-catalyst, which increases the production cost

Method used

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  • Phase-transfer catalyst quaternary ammonium salt and preparation method thereof
  • Phase-transfer catalyst quaternary ammonium salt and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0017] Put 20.54g of 1-bromobutane, 10.65g of dimethyl dodecyl tertiary amine, 0.7mol of ethanol into a 250mL single-necked bottle, raise the temperature to 70°C, stir at reflux for 24h, and analyze by TLC (methanol:chloroform=2:10) , dimethyl dodecyl tertiary amine point disappears. The solvent and unreacted 1-bromobutane were distilled off under reduced pressure. A white solid was obtained: 16.48 g of dimethyl n-butyl n-dodecyl ammonium bromide. The yield is 94.2%

Embodiment 2

[0019] 20.54g of 1-bromobutane, 12.05g of dimethyltetradecyl tertiary amine, 32g of ethanol were added into a 250mL single-necked bottle, raised to 70°C, stirred at reflux for 24h, analyzed by TLC (methanol:chloroform=2:10), The tertiary dimethyltetradecylamine point disappears. The solvent and unreacted 1-bromobutane were distilled off under reduced pressure. Obtained white solid: dimethyl n-butyl n-tetradecyl ammonium bromide 17.59g, yield 93.1%

Embodiment 3

[0021] 18.45g of 1-bromopropane, 13.45g of dimethylhexadecyl tertiary amine, 32g of ethanol were put into a 250mL single-necked bottle, raised to 70 degrees, stirred at reflux for 24h, analyzed by TLC (methanol:chloroform=2:10), two The methyl hexadecyl tertiary amine point disappears. The solvent and unreacted 1-bromopropane were distilled off under reduced pressure. A white solid was obtained: 18.61 g of dimethyl n-propyl n-hexadecyl ammonium bromide, and the yield was 95%.

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Abstract

The invention relates to phase-transfer catalyst quaternary ammonium salt and a preparation method thereof. The preparation method is characterized in that: the quaternary ammonium salt is prepared by the reaction between haloalkane and aliphatic amine in an organic solvent. The phase-transfer catalyst has high catalytic activity; and the preparation method is simple, can effectively improve the product yield and content of a cycloaliphatic epoxy resin synthesizing process, and simplifies the synthesizing process, so that the synthesizing process is more environment-friendly and safe, and the production cost can be reduced. The phase-transfer catalyst quaternary ammonium salt is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a phase transfer catalyst used in the synthesis process of alicyclic epoxy resin, in particular to a quaternary ammonium salt phase transfer catalyst and a preparation method thereof. Background technique [0002] Epoxy resin is an important thermosetting resin variety, which is widely used in chemical industry, light industry, water conservancy, transportation, machinery, electronics, home appliances, automobiles, aerospace and other industrial fields. Alicyclic epoxy resins are usually a class of epoxy compounds obtained by oxidizing corresponding unsaturated alicyclic compounds with peroxidic organic acids. Its structural feature is that it contains an alicyclic ring, and the epoxy group is directly connected to the alicyclic ring. As a new generation of epoxy resin, alicyclic epoxy resin has excellent electrical properties such as arc resistance, high volume resistance and surface resistance due to its structural characteri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63B01J31/02C07D301/12C07D303/48
Inventor 杨建宇徐波常杨军
Owner JIANGSU TETRA NEW MATERIAL TECH
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