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Preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate

A technology of pentanediol monoisobutyrate and trimethyl is applied in the field of preparation of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and can solve the problem of decreasing catalytic activity , difficult distillation separation and other problems, to achieve the effect of less catalyst dosage, good selectivity and mild reaction conditions

Inactive Publication Date: 2020-11-03
武汉昱鼎科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This separation method needs to introduce water, and water and isobutyraldehyde form an azeotrope, which is difficult to separate by rectification. In addition, the catalytic activity of the inorganic base catalyst generated after washing with water is significantly lower than that of organic bases.

Method used

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  • Preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate
  • Preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate
  • Preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate

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Embodiment 1

[0038] A preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, comprising the following steps:

[0039] S1. In a 500ml three-neck flask equipped with a reflux condenser and a stirrer, add 100g isobutyraldehyde (1.389mol), and ionic liquid catalyst A, 10g, stir, and the reaction pressure is 0.5MPa;

[0040] S2. The temperature of the reaction system was raised to 65° C., and the stirring reaction was continued for 2 h.

[0041] S3. Cool the reaction system to room temperature, remove unreacted raw materials, and then separate by vacuum distillation to obtain 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate.

Embodiment 2

[0043] A preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, comprising the following steps:

[0044] S1. In a 500ml three-neck flask equipped with a reflux condenser and a stirrer, add 100g isobutyraldehyde (1.389mol), and ionic liquid catalyst B, 12.7g, stir, and the reaction pressure is 0.5MPa;

[0045] S2. The temperature of the reaction system was raised to 65° C., and the stirring reaction was continued for 2 h.

[0046] S3. Cool the reaction system to room temperature, remove unreacted raw materials, and then separate by vacuum distillation to obtain 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate.

Embodiment 3

[0048] A preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, comprising the following steps:

[0049] S1. In a 500ml three-neck flask equipped with a reflux condenser and a stirrer, add 100g isobutyraldehyde (1.389mol), and ionic liquid catalyst C, 20.3g, stir, and the reaction pressure is 0.5MPa;

[0050] S2. The temperature of the reaction system was raised to 65° C., and the stirring reaction was continued for 2 h.

[0051] S3. Cool the reaction system to room temperature, remove unreacted raw materials, and then separate by vacuum distillation to obtain 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate.

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Abstract

The invention relates to the technical field of organic synthesis, in particular to a method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. According to the method, isobutyraldehyde issubjected to a condensation reaction in the presence of an ionic liquid catalyst to obtain 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. An ionic liquid the cation of which is alkyl imidazole cations or benzimidazole cations and the anion of which is at least one of hydroxyl ions and acetate ions is adopted as the catalyst. The 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate.is prepared through one step, the reaction conditions are mild, the reaction conversion rate is high, selectivity is good, and subsequent products are easy to separate.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate, commonly known as alcohol ester dodeca, also known as Texanol alcohol ester, is a water-insoluble high-boiling diol Ester has good resin compatibility, viscosity, good film-forming performance, low melting point, and can effectively reduce the film-forming temperature of high glass transition temperature emulsion paints. It has been widely used as a film-forming aid for coatings. [0003] At present, the industrial production of alcohol ester twelve is to use isobutyraldehyde as raw material, under the action of basic catalyst, undergo aldol condensation, Cannizzaro reaction, and then separate to obtain the product. At present, the commonly used catalysts are inorganic bases, especially alkali metal hydroxides are the m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/44C07C69/28B01J31/02
CPCB01J31/0284C07C67/44C07C69/28
Inventor 崇明本冯建成冯子涵袁野
Owner 武汉昱鼎科技有限公司
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