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Preparation method of six-membered glyceryl acetal

A technology of hexavalent glycerol and glycerin acetal, which is applied in organic chemistry methods, organic chemistry, etc., can solve the problems of poor reactivity, high viscosity of glycerin, and low product yield, and achieve the effect suitable for popularization and use

Inactive Publication Date: 2019-08-23
NANJING VSKY GREENCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Glycerin has high viscosity and strong polarity, and there is a difference in polarity with aliphatic aldehydes. The two are incompatible with each other, which makes the condensation reaction of glycerol and aliphatic aldehydes have problems such as poor reactivity and low product yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of preparation method of six yuan glycerol acetal that the present invention proposes, comprises the following steps,

[0019] S1, including the following molar parts of raw materials: 10 parts of glycerin, 4 parts of n-octylaldehyde, 4 parts of lauryl aldehyde, and 5 parts of catalyst;

[0020] S2, put the above-mentioned molar parts of glycerin, n-octylaldehyde, laurylaldehyde, and catalyst into the reaction kettle at the same time, the reaction temperature is 45°C, and the reaction time is 5h, to obtain cis six-membered ring glycerol acetal, trans six-membered ring Glycerol acetal, cis five-membered ring glycerol acetal and trans five-membered ring glycerol acetal mixture;

[0021] S3, the mixture of cis six-membered ring glycerol acetal, trans six-membered ring glycerol acetal, cis five-membered ring glycerol acetal and trans five-membered ring glycerol acetal is separated by a rectifying column to obtain The separated cis six-membered ring glycerol acetal, ...

Embodiment 2

[0024] A kind of preparation method of six yuan glycerol acetal that the present invention proposes, comprises the following steps,

[0025] S1, including the following molar parts of raw materials: 11.5 parts of glycerin, 5 parts of n-octylaldehyde, 5 parts of lauryl aldehyde, and 6 parts of catalyst;

[0026] S2, put the above-mentioned molar parts of glycerin, n-octylaldehyde, laurylaldehyde, and catalyst into the reaction kettle at the same time, the reaction temperature is 50°C, and the reaction time is 5.5h to obtain cis six-membered ring glycerol acetal, trans six-membered Cycloglycerol acetal, cis five-membered ring glycerol acetal and trans five-membered ring glycerol acetal mixture;

[0027] S3, the mixture of cis six-membered ring glycerol acetal, trans six-membered ring glycerol acetal, cis five-membered ring glycerol acetal and trans five-membered ring glycerol acetal is separated by a rectifying column to obtain The separated cis six-membered ring glycerol aceta...

Embodiment 3

[0030] A kind of preparation method of six yuan glycerol acetal that the present invention proposes, comprises the following steps,

[0031] S1, including the following molar parts of raw materials: 13 parts of glycerin, 6 parts of n-octylaldehyde, 6 parts of lauryl aldehyde, and 7 parts of catalyst;

[0032] S2, put the above molar parts of glycerin, n-octylaldehyde, lauryl aldehyde, and catalyst into the reaction kettle at the same time, the reaction temperature is 55°C, and the reaction time is 6h, to obtain cis six-membered ring glycerol acetal, trans six-membered ring Glycerol acetal, cis five-membered ring glycerol acetal and trans five-membered ring glycerol acetal mixture;

[0033] S3, the mixture of cis six-membered ring glycerol acetal, trans six-membered ring glycerol acetal, cis five-membered ring glycerol acetal and trans five-membered ring glycerol acetal is separated by a rectifying column to obtain The separated cis six-membered ring glycerol acetal, trans six...

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PUM

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Abstract

The invention belongs to the technical field of preparation of six-membered glyceryl acetal, and in particular discloses a preparation method of the six-membered glyceryl acetal. The method comprisesthe following steps: step 1, preparing the following raw materials, in parts by molar: 10-13 parts of glycerin, 4-6 parts of n-octanal, and 5-7 parts of a catalyst; step 2, simultaneously adding the glycerin, the n-octanal, lauraldehyde and the catalyst into a reaction kettle according to the above molar by parts, performing a reaction for 5-6 h at reaction temperature of 45-55 DEG C to obtain a mixture of cis six-membered cyclic glyceryl acetal, cis five-membered cyclic glyceryl acetal and trans five-membered cyclic glyceryl acetal; and step 3, performing separation on the cis six-membered cyclic glyceryl acetal, trans six-membered cyclic glyceryl acetal, the cis five-membered cyclic glyceryl acetal and the trans five-membered cyclic glyceryl acetal by using a rectification column. According to the method provided by the invention, the six-membered cyclic glyceryl acetal and the derivatives of the six-membered cyclic glyceryl acetal prepared by the method are applied in the field of decomposable surfactants and degradable bio-based lubricating oil, the yield can be up to 98.8%, and the method is suitable for promotion and use.

Description

technical field [0001] The invention relates to the technical field of preparing hexavalent glycerol acetal, in particular to a preparation method of hexavalent glycerol acetal. Background technique [0002] Glycerol acetal or ketal compounds are an important class of fine chemicals synthesized from glycerol and aldehydes or ketones through acetal or ketal reactions, and have potential applications in the fields of fuel additives, surfactants, lubricant additives, solvents, etc. application value. The fatty aldehyde glycidol synthesized by the acetal reaction of glycerol and aliphatic aldehyde is an important hydrophobic intermediate for the synthesis of decomposable surfactants. Glycerol has high viscosity and strong polarity, and there is a difference in polarity with aliphatic aldehydes. The two are incompatible with each other, which makes the condensation reaction of glycerol and aliphatic aldehydes have problems such as poor reactivity and low product yield. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06C07D317/12
CPCC07B2200/09C07D317/12C07D319/06
Inventor 不公告发明人
Owner NANJING VSKY GREENCHEM
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