Environment-friendly preparation method of pentaerythritol acrylic ester and derivate

A technology of pentaerythritol acrylate and derivatives, which is applied in the field of acrylate synthesis, can solve the problems of poor catalyst cycle performance, complicated post-treatment process, and low product yield, so as to avoid discharge of salty wastewater, easy recycling, and high yield high effect

Active Publication Date: 2013-09-04
CHANGZHOU XIAOGUO INFORMATION SERVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is: in the preparation method of pentaerythritol acrylate and its derivatives in the prior art, there are problems of low product yield, serious pollution, complicated post-treatment process, and poor catalyst cycle performance

Method used

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  • Environment-friendly preparation method of pentaerythritol acrylic ester and derivate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Put 1,650g (95%) of pentaerythritol, 1,500g of cyclohexane, 2,550g of acrylic acid, and 55g of silica gel functionalized with sulfonic acid group into the reactor with reflux water separator, (the structure is as above, the catalyst of structural formula C-1 , n=1, its average pore diameter is 18.3nm, and its specific surface area is 480m 2 / g, sulfo group (SO 3 H) Functionalized density is 5gSO 3 H / 100g silica gel), p-hydroxyanisole 8g. Reflux dehydration esterification reaction for 10.8 hours, and 625 g of water was separated. Stop heating and reflux, and cool down to 50°C;

[0025] (2) Recover the C-1 catalyst by filtration. Under the situation of vigorous stirring, add quicklime to total 56g in the filtrate gradually, make material pH=6, then add magnesium polysilicate 70g, stir again 0.5 hour;

[0026] (3) Finally, decyclohexane was removed under reduced pressure at 60°C and suction filtered to obtain 3249 g of pentaerythritol triacrylate, a light yellow, ...

Embodiment 2

[0029] (1) Put 1650g (95%) of pentaerythritol, 1500g of benzene, 2550g of acrylic acid, and 127g of aluminum gel functionalized with sulfonic acid group into the reactor with reflux water separator (the structure is as above, the catalyst of structural formula C-2, n= 3. The average pore diameter is 14.2nm and the specific surface area is 210m 2 / g, sulfo group (SO 3 H) The functionalized density is 15gSO 3 H / 100g aluminum glue), hydroquinone 2.6g. Reflux dehydration esterification reaction for 7.5 hours, and 621 g of water was separated. Stop heating and reflux, and cool down to 50°C.

[0030] (2) Recover the C-2 catalyst by filtration. In the case of strong stirring, gradually add a total of 87g of alkaline calcium-based bentonite to the filtrate to make the material pH=6, then add 60g of activated carbon, and stir for another 0.5 hours.

[0031] (3) Finally, debenzene was removed under reduced pressure at 60°C and suction filtered to obtain 3228 g of pentaerythritol tr...

Embodiment 3

[0034] (1) Put 1650g (95%) of pentaerythritol (95%), 1200g of isopropyl ether, 2550g of acrylic acid, and 250g of silica gel functionalized with sulfonic acid group into the reactor with reflux water separator (the structure is as above, the catalyst of structural formula C-3, n =2, the average pore diameter is 10.5nm, and the specific surface area is 360m 2 / g, sulfo group (SO 3 H) The functionalized density is 30gSO 3 H / 100g silica gel), phenothiazine 32.3g, copper sulfate 4g. Reflux dehydration and esterification for 4.5 hours, and 630 g of water was separated. Stop heating and reflux, and cool down to 50°C.

[0035] (2) Recover the C-3 catalyst by filtration. Under the condition of vigorous stirring, gradually add 27g of sodium bicarbonate in total to the filtrate to make the material pH=6~7, then add 95g of alkaline calcium-based bentonite, and stir for another 0.5 hour.

[0036] (3) Finally, deisopropyl ether was removed under reduced pressure at 60°C, and suction fil...

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Abstract

The invention belongs to a preparation method of pentaerythritol acrylic ester and a derivate. The method comprises the following steps of: in the presence of solvents and polymerization inhibitors, catalyzing pentaerythritol (or dipentaerythritol) and acrylic acid by using a chemical binding solid acid catalyst to perform a backflow dehydration esterification reaction; after the reaction is finished, filtering and recycling the chemical binding solid acid catalyst, and then, processing a product by using a solid alkali adsorbent and a decolorizing agent; and finally, performing pressure reduction and filtering to obtain pentaerythritol (or dipentaerythritol) acrylic ester. The preparation method is simple in process, high in yield of the product and high in quality; and wastewater discharge is avoided during production, and the catalyst is recycled.

Description

technical field [0001] The invention belongs to the field of acrylate synthesis, in particular to a preparation method of pentaerythritol acrylate and derivatives. Background technique [0002] Both pentaerythritol acrylate and dipentaerythritol acrylate are important polyfunctional polymerization monomers. For example: pentaerythritol triacrylate is a monomer containing a side hydroxyl group, low volatility, fast curing, mainly used for free radical polymerization. It can give coatings: weather resistance, water resistance, chemical resistance, high adhesion, high hardness, wear resistance and heat resistance. Can be used in elastomers, sealants, fluxes, adhesives, glass, metal, floor coatings, wood and paper coatings and inks. Dipentaerythritol pentaacrylate is an important multifunctional monomer and diluent. It has the advantages of high double bond content, fast curing speed, and excellent cured film performance. It is widely used in photocurable inks, coatings, and e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/08B01J31/02
CPCY02P20/584
Inventor 单玉华高秋敏曹鹰常彬彬栾宁万宇司坤坤
Owner CHANGZHOU XIAOGUO INFORMATION SERVICES
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