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2,2,4-trimethyl pentanediol monoester synthesizing method

A technology of trimethylpentanediol monoester and synthesis method, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of dehydration reaction of synthetic raw materials and low selectivity of synthesis reaction, etc. Improve selectivity and inhibit dehydration reaction

Inactive Publication Date: 2018-03-20
RUNTAI CHEM TAIXING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the existing synthetic method, due to the reaction under acidic conditions, the synthetic raw material is very prone to dehydration reaction, so that the prepared mixture contains a large amount of double bonds, and the selectivity of the synthetic reaction is low

Method used

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  • 2,2,4-trimethyl pentanediol monoester synthesizing method
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  • 2,2,4-trimethyl pentanediol monoester synthesizing method

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preparation example Construction

[0019] A kind of synthetic method of 2,2,4-trimethylpentanediol monoester, described synthetic method comprises the following steps:

[0020] In the presence of an acidic catalyst, the alkyl aldehyde compound undergoes a condensation reaction for 1-5 hours;

[0021] The obtained mixture is separated and purified to obtain 2,2,4-trimethylpentanediol monoester;

[0022] The acidic catalyst is a mixture of oxalic acid and molecular sieve, the molecular sieve is a zeolite molecular sieve, and the surface of the zeolite molecular sieve has proton acid sites;

[0023] The structure of the alkyl aldehyde compound is as follows:

[0024]

[0025] The structure of the 2,2,4-trimethylpentanediol monoester is as follows:

[0026]

[0027] The R 1 , R 2 For methyl.

[0028] The molecular sieve of the present invention is a porous body having pores with uniform pore diameters. Among them, the form of molecular sieve zeolite and molecular sieve activated carbon is not particular...

Embodiment 1

[0054]In a reactor equipped with a condenser, a stirring device, and a thermometer, add 2g of 2,2,4-trimethylpentanediol monoester HY type zeolite (H-ZSM-52,2,4-trimethylpentanediol Monoester, exchange degree 90%, SiO2 / Al2O3 molar ratio 18) and 0.05g oxalic acid, add 200g isobutyraldehyde for condensation reaction, control the reaction temperature at 70-80 degrees Celsius, react at 70-80 degrees Celsius for 25 minutes, heat up To 100 degrees Celsius, the reaction temperature is controlled at 100-110 degrees Celsius, and the reaction is carried out at 100-110 degrees Celsius for 50 minutes to prepare a synthetic liquid. Under reduced pressure distillation under the condition of -0.097MPa, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was obtained. Analyzing the synthesis solution, the conversion rate of isobutyraldehyde was 86.9%, and the selectivity of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was 96.9%.

Embodiment 2

[0056] In a reactor equipped with a condenser, a stirring device, and a thermometer, add 2g of 2,2,4-trimethylpentanediol monoester HY type zeolite (H-ZSM-52,2,4-trimethylpentanediol Monoester, exchange degree 90%, SiO2 / Al2O3 molar ratio 23) and 0.1g oxalic acid, add 200g isobutyraldehyde for condensation reaction, control the reaction temperature at 70-80 degrees Celsius, react at 70-80 degrees Celsius for 25 minutes, heat up To 100 degrees Celsius, the reaction temperature is controlled at 100-110 degrees Celsius, and the reaction is carried out at 100-110 degrees Celsius for 40 minutes to prepare a synthetic liquid. Under reduced pressure distillation under the condition of -0.097MPa, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was obtained. Analyzing the synthesis liquid, the conversion rate of isobutyraldehyde was 88.3%, and the selectivity of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was 96.2%.

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Abstract

The invention relates to a 2,2,4-trimethyl pentanediol monoester synthesizing method. The synthesizing method comprises the following steps: under existence of an acid catalyst, performing condensation reaction on an alkyl aldehyde compound for 1 to 5 hours; separating and purifying an obtained mixture to obtain 2,2,4-trimethyl pentanediol monoester, wherein the acid catalyst is a mixture of oxalic acid and a molecular sieve, the molecular sieve is a zeolite molecular sieve, and the surface of the zeolite molecular sieve has a protonic acid site. According to the 2,2,4-trimethyl pentanediol monoester synthesizing method, a specific catalyst is utilized, so that dehydration reaction is greatly inhibited, and reaction selectivity is greatly improved.

Description

technical field [0001] The invention relates to a method for synthesizing 2,2,4-trimethylpentanediol monoester. Background technique [0002] With the rapid development of my country's construction and decoration industry, people's requirements for quality of life are constantly improving and with the continuous enhancement of environmental protection awareness, the coating industry has further strictly controlled the content of VOC (volatile organic compounds with a boiling point below 250 ° C), as Water-based latex paint, one of the decorative materials, has become the main material for building interior wall decoration, while the application rate of building exterior wall decoration has reached 35%. Many latex polymers used in latex paints cannot form films at room temperature, because most latex polymers cannot form films at low temperatures. In order to make the latex paint form a complete film, it is necessary to add a coalescent film-forming aid. Coalescents are usua...

Claims

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Application Information

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IPC IPC(8): C07C67/39C07C69/28
CPCC07C67/39C07C69/28
Inventor 张海飞杨萍宋文娟薛和太
Owner RUNTAI CHEM TAIXING CO LTD
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