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Preparation method of pentaerythritol ester

A technology for pentaerythritol ester and pentaerythritol is applied in the field of preparation of pentaerythritol ester, and can solve the problems of many by-products, difficult recycling of catalysts, and difficulty in achieving industrial application.

Pending Publication Date: 2020-10-27
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, inorganic acid has the advantages of low price and high activity, but it is easy to corrode the reaction equipment in the synthesis, and there are many by-products, which will pollute the environment with a large amount of waste acid.
Organic acid catalysts such as p-toluenesulfonic acid do not corrode equipment and cause little pollution to the environment, but they belong to a homogeneous reaction. The catalyst is difficult to recycle and the post-processing of the product is difficult.
[0007] In addition, the yield of the above reaction is low, it is difficult to meet the needs of industrial applications

Method used

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  • Preparation method of pentaerythritol ester
  • Preparation method of pentaerythritol ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1. Catalyst H 3 PW 12 o 40 -Methanesulfonic acid / Mesoporous TiO 2 Preparation of:

[0057] A) 30.5 g of template agent P12 and 5 g of isopropyl titanate were stirred in ethanol for 1 h and mixed evenly to obtain the first mixed solution;

[0058] B) the first mixed solution and heteropolyacid H 3 PW 12 o 40 1 g, 1 g of methanesulfonic acid were stirred for 1 h and mixed uniformly to obtain the second mixed solution;

[0059] C) volatilize the second mixed solution at 40° C. for 12 hours to remove the solvent to obtain a gel;

[0060]D) Aging at 100°C for 12h, and then calcining at 350°C for 2h to remove the template agent and obtain catalyst H 3 PW 12 o 40 -Methanesulfonic acid / Mesoporous TiO 2 . The particle size of the catalyst is 3nm and the specific surface area is 200m 2 / g.

[0061] 2, the preparation of pentaerythritol ester

[0062] (1) In the four-neck flask equipped with mechanical stirring, thermometer, reflux condenser and water trap, add 41.2...

Embodiment 2

[0072] 1. Catalyst H 3 SiW 12 o 40 -Sulphamic acid / mesoporous TiO 2 Preparation of:

[0073] A) 31 g of template agent P12 and 8 g of n-butyl titanate were stirred in methanol for 0.5 h and mixed uniformly to obtain the first mixed solution;

[0074] B) the first mixed solution and heteropolyacid H 3 SiW 12 o 40 3g, 1g of sulfamic acid were stirred for 1h and mixed uniformly to obtain the second mixed solution;

[0075] C) volatilize the second mixed solution at 40° C. for 13 hours to remove the solvent to obtain a gel;

[0076] D) Aging at 100°C for 14h, and then calcining at 400°C for 2h to remove the template agent to obtain catalyst H 3 SiW 12 o 40 -Sulphamic acid / mesoporous TiO 2 . The particle size of the catalyst is 3.5nm and the specific surface area is 180m 2 / g.

[0077] 2, the preparation of pentaerythritol ester

[0078] (1) In the four-necked flask that mechanical stirring, thermometer, reflux condenser and water separator are housed, add 41.27g of ...

Embodiment 3

[0086] 1. Catalyst H 3 PW 12 o 40 -Methanesulfonic acid / mesoporous SiO 2 Preparation of:

[0087] A) 30.8 g of template agent P12 and 7 g of ethyl orthosilicate were stirred in acetonitrile for 1.5 h and mixed uniformly to obtain the first mixed solution;

[0088] B) the first mixed solution and heteropolyacid H 3 PW 12 o 40 2g and 2g of methanesulfonic acid were stirred for 1h and mixed uniformly to obtain the second mixed solution;

[0089] C) volatilize the second mixed solution at 40° C. for 10 h to remove the solvent to obtain a gel;

[0090] D) aging at 100°C for 12h, and then calcining at 400°C for 1.5h to remove the template agent and obtain catalyst H 3 PW 12 o 40 -Methanesulfonic acid / mesoporous SiO 2 . The particle size of the catalyst is 4nm and the specific surface area is 210m 2 / g.

[0091] 2, the preparation of pentaerythritol ester

[0092] (1) In the four-neck flask equipped with mechanical stirring, thermometer, reflux condenser and water sepa...

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Abstract

The invention provides a preparation method of pentaerythritol ester. The preparation method comprises the following steps: carrying out esterification reaction on pentaerythritol and 3-mercaptobutyric acid under the action of a catalyst to generate pentaerythritol tetra (3-mercaptobutyric acid) ester; the catalyst is prepared by the following method: A) uniformly mixing a template agent and a titanium source compound or a silicon source compound in a solvent to obtain a first mixed solution; B) uniformly mixing the first mixed solution with heteropoly acid and an organic compound with a sulfonic acid group to obtain a second mixed solution; C) removing the solvent from the second mixed solution to obtain gel; and D) carrying out aging treatment on the gel, and roasting to remove the template agent to obtain the catalyst. The supported composite acid catalyst is adopted to synthesize pentaerythritol tetra (3-mercaptobutyric acid) ester, inorganic acid and organic acid catalysts are replaced, the catalyst has higher acidity and catalytic activity, the esterification efficiency can be improved, the reaction time can be shortened, and the catalyst can be repeatedly used and is greener, more environmentally friendly and more economical.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of pentaerythritol ester. Background technique [0002] Photocuring technology is known as a "green" technology. Mercapto-ene photocuring systems are widely used in coatings, adhesives, photoresists, photosensitive materials and 3D printing. The addition of mercapto groups can effectively solve the problem of surface oxygen inhibition of traditional acrylate systems. However, the currently used mercapto monomers are all primary mercaptans, which have problems such as poor storage stability and strong odor. [0003] Pentaerythritol tetrakis (3-mercaptobutyrate) ester is an important chemical and organic synthesis intermediate, with low odor, and can form a highly stable mercapto-ene formula. Mainly used in UV curing glue, UV ink, epoxy curing agent, etc. [0004] At present, pentaerythritol tetrakis (3-mercaptobutyrate) ester is generally prepare...

Claims

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Application Information

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IPC IPC(8): C07C319/12C07C323/52B01J31/18B01J35/02B01J35/10
CPCC07C319/12B01J27/188B01J31/38B01J31/0225B01J27/24B01J35/40B01J35/615C07C323/52
Inventor 许倩倩梁万根张超崔卫华费潇瑶孙志利卞文
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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