Method for synthesizing 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate) by adopting micro-channel reactor

A technology of pentanediol monoisobutyrate and microchannel reactor, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, carboxylate preparation, etc., to achieve precise controllable temperature and precise reaction conditions Controllable, great results

Inactive Publication Date: 2020-06-26
CHANGZHOU VOCATIONAL INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] So far, it has not been seen that the reaction of isobutyraldehyde in the presence of a composite catalyst (alkali metal hyd

Method used

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  • Method for synthesizing 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate) by adopting micro-channel reactor
  • Method for synthesizing 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate) by adopting micro-channel reactor
  • Method for synthesizing 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate) by adopting micro-channel reactor

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Embodiment 1

[0027] The method for synthesizing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate using a microchannel reactor of the present invention, using isobutyraldehyde as a raw material, and brominating with sodium hydroxide and tetrabutyl The composite solution of ammonium configuration is a composite catalyst solution, and 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate is synthesized in a microchannel reactor (see attached figure 1 ), including the following steps:

[0028] S1: Configuration of the composite catalyst solution, dissolving sodium hydroxide and tetrabutylammonium bromide in deionized water to form a composite catalyst solution of a certain concentration, wherein the mass concentration of sodium hydroxide is 20%, tetrabutylammonium bromide The mass concentration is 0.6%;

[0029] S2: The setting of the reaction conditions of the microchannel reactor, the heat exchange sheet integrated with the reaction sheet in the microchannel reactor is connected to the external he...

Embodiment 2

[0033]The method for synthesizing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate using a microchannel reactor of the present invention, using isobutyraldehyde as a raw material, and brominating with potassium hydroxide and tetrabutyl The composite solution configured by ammonium is a composite catalyst solution, and 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate is synthesized in a microchannel reactor, including the following steps:

[0034] S1: Configuration of the composite catalyst solution, dissolving potassium hydroxide and tetrabutylammonium bromide in deionized water to form a composite catalyst solution of a certain concentration, wherein the mass concentration of potassium hydroxide is 30%, tetrabutylammonium bromide The mass concentration is 1%;

[0035] S2: The setting of the reaction conditions of the microchannel reactor, the heat exchange sheet integrated with the reaction sheet in the microchannel reactor is connected to the external heating and cooling circu...

Embodiment 3

[0039] The method for synthesizing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate using a microchannel reactor of the present invention, using isobutyraldehyde as a raw material, and brominating with potassium hydroxide and tetrabutyl The composite solution configured by ammonium is a composite catalyst solution, and 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate is synthesized in a microchannel reactor, including the following steps:

[0040] S1: Configuration of the composite catalyst solution, dissolving potassium hydroxide and tetrabutylammonium bromide in deionized water to form a composite catalyst solution of a certain concentration, wherein the mass concentration of potassium hydroxide is 10%, tetrabutylammonium bromide The mass concentration is 0.8%;

[0041] S2: The setting of the reaction conditions of the microchannel reactor, the heat exchange sheet integrated with the reaction sheet in the microchannel reactor is connected to the external heating and cooling ci...

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Abstract

The invention discloses a method for synthesizing 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate) by adopting a micro-channel reactor and relates to the technical field of organic synthesis application. The method comprises the four steps: preparing a composite catalyst solution; setting reaction conditions of a micro-channel reactor; synthesizing 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate); and performing post treatment. According to the method, isobutyraldehyde is used as a raw material, and alkali metal hydroxide and tetrabutylammonium bromide are used as a composite catalyst; the 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate) is synthesized in the micro-channel reactor in a continuous flow manner. Compared with the prior art, the method disclosed by the invention has the characteristics of accurate and controllable reaction conditions, continuous production mode, high safety and short reaction time, the isobutyraldehyde conversion rate reaches over 95%,few reaction byproducts are produced, the selectivity reaches 80-95%, and the target product yield reaches 76-85%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis applications, and in particular relates to a method for synthesizing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate using a microchannel reactor. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate is a water-insoluble diol ester with high boiling point and low freezing point. It has very good compatibility with various solvents. And it is non-toxic, and it is generally recognized as a green solvent, widely used in coating film-forming aids, synthetic lubricants, plasticizers and other fields. [0003] In the prior art, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate adopts a batch or continuous production process, and due to uneven mixing of reaction materials, it is easy to cause local catalyst concentration to be too high or Problems such as too low, thereby cause side reaction to increase, product yield is low, the disadvantages such as product purity is n...

Claims

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Application Information

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IPC IPC(8): C07C67/00C07C69/28B01J19/00
CPCC07C67/00B01J19/0093
Inventor 王晓东乔奇伟李莹雪宋智谦李英利蒋涛李艳秋李树白
Owner CHANGZHOU VOCATIONAL INST OF ENG
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