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Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate

A technology of pentanediol monoisobutyrate and trimethyl, applied in the field of preparation 2, can solve the problems of low isobutyraldehyde conversion rate target product selectivity, high quality requirements, no industrialization prospects, etc., and avoids the reaction process. Complicated, high yield per pass and less catalyst dosage

Active Publication Date: 2011-01-19
YIXING HENGXING FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] Patent CN01140554.6 adopts a one-stage reaction process, that is, aldol condensation and Cannizzaro reaction are carried out simultaneously in the same reactor, but the catalyst is poisonous Ba(OH) 2 , and this process has high requirements on the quality of raw materials. When isobutyraldehyde contains water and isobutyric acid, the conversion rate of isobutyraldehyde and the selectivity of target products are low, and there is no industrialization prospect

Method used

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  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate

Examples

Experimental program
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Embodiment 1

[0021] Embodiment 1, in the 500ml there-necked flask that is equipped with reflux condenser and stirring, add 200g isobutyraldehyde (2.778mol), catalyzer is dry solid sodium methylate powder 3.75g (0.0694mol), and sodium methylate is added intermittently, will The temperature of the reaction system was raised to 60° C., and the stirring reaction was continued for 2 h, and the reaction was carried out under normal pressure. Then it was cooled to room temperature, washed with water, and the reaction mixture was analyzed, and the conversion rate of isobutyraldehyde was 73%. Unreacted isobutyraldehyde was removed under reduced pressure, and the crude product was analyzed. The alcohol ester dodecane content was 97%, the by-product TXIB content was about 2%, and other components accounted for about 1%, of which 2,2,4-trimethyl -1,3-pentanediol content is very small. The crude product is then separated by vacuum distillation, and more than 99.5% of the finished product of alcohol es...

Embodiment 2

[0023] Example 2, the reaction device, isobutyraldehyde and its dosage are the same as in Example 1, the catalyst is 3 g (0.0556 mol) of sodium methoxide, the sodium methoxide is added intermittently, and the temperature of the reaction system is raised to 70° C., and the stirring reaction is continued for 1 h. Aftertreatment and product analysis are the same as in Example 1.

Embodiment 3

[0024] Example 3, the reaction device, isobutyraldehyde and its dosage are the same as in Example 1, the catalyst is 1 g (0.0185 mol) of sodium methoxide, sodium methoxide is added intermittently, and then the temperature of the reaction system is raised to 80° C., and the reaction is continued for 0.5 h with stirring. Aftertreatment and product analysis are the same as in Example 1.

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Abstract

The invention discloses a method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, which relates to the technical field of organic synthesis. In the invention, isobutylaldehyde is used as a raw material, aldol condensation and Cannizzaro reactions are completed by a one-step reaction process in the presence of a catalyst, and the process adopts sodium alcoholate as the catalyst; and the isobutylaldehyde is used to form alcohol ester-12 in the presence of the sodium alcoholate catalyst, so the complex and high-energy consumption drawbacks of a two-step reaction process using an inorganic alkali as a catalyst are overcome, the drawbacks of toxic catalyst and high quality requirement on the isobutylaldehyde raw material of a one-step reaction process using Ba(OH)2 as a catalyst are overcome, and simple process, high single-pass yield, small catalyst dosage, low energy consumption, safety and environmental protection are realized.

Description

technical field [0001] 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 by using isobutyraldehyde as a raw material and using sodium alkoxide as a catalyst. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate, also known as alcohol ester dodecyl or Texanol alcohol ester, is a water-insoluble high-boiling glycol ester, because of its It has good resin compatibility and viscosity, good film-forming performance, low freezing point, and can effectively reduce the film-forming temperature of high glass transition temperature latex paint. It has been widely used as a new coating film forming aid for coatings. Alcohol ester twelve can improve the weather resistance, cleanability, touch-up and color development of the coating, etc., and has low toxicity, low dosage and good hydrolytic stability. It is a safe and efficient A new type of green film-formi...

Claims

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Application Information

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IPC IPC(8): C07C69/28C07C67/44
Inventor 崇明本张千卢荣群何珍娟陈维斌王恒秀张剑彬
Owner YIXING HENGXING FINE CHEM
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