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Preparation method of high-purity (bi)pentaerythritol crylic acid non-complete esterification product

A technology of pentaerythritol acrylic acid and pentaerythritol, which is applied in the field of acrylate synthesis, can solve the problems of low product purity, and achieve the effect of high purity and good product performance

Active Publication Date: 2013-08-21
CHANGZHOU XIAOGUO INFORMATION SERVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the later stage of the reaction, due to the relative shortage of acrylic acid, the esterification rate of the generated product will be lower than that of the target product.
This results in lower product purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 1650g (95%) of pentaerythritol (95%) and 4950g of dioxane into the reactor with reflux water separator, heat to reflux at 105°C, wait until the pentaerythritol is basically dissolved, add 2500g of acrylic acid, 126g of p-toluenesulfonic acid, and 5g of hydroquinone . The reaction system was heated to 105°C, and 4900 g of dioxane was distilled off (because dioxane will be distilled out together with water and is completely miscible with water). Subsequently, 1500 g of cyclohexane was added into the reactor. Reflux dehydration esterification at 85°C for 6.5 hours, and 602 g of water was separated. Stop heating and reflux, and cool down to 50°C. Under the condition of vigorous stirring, gradually add saturated sodium carbonate solution to make the material pH=7, separate the water layer, and then wash the organic layer with distilled water three times to make the material neutral. Finally, the solvent was removed under reduced pressure and suction filtered to obtain...

Embodiment 2

[0019] Put 1650g (95%) of pentaerythritol (95%) and 2475g of water into the reactor with reflux water separator, heat to reflux at 100°C, wait until the pentaerythritol is basically dissolved, add 1798g of acrylic acid, 86g of methanesulfonic acid, 13.8g of p-hydroxyanisole, benzene 1500g. 80°C reflux dehydration esterification reaction for 8.6 hours, a total of 2876g of water was separated. Stop heating and reflux, and cool down to 50°C. Under the condition of vigorous stirring, gradually add saturated sodium carbonate solution to make the material pH=8, separate the water layer, and then wash the organic layer with distilled water three times to make the material neutral. Finally, the solvent was removed under reduced pressure and suction filtered to obtain 2424.4 g of a slightly yellow, transparent viscous liquid product (yield about 86.4%). High-pressure liquid chromatography analysis product content is: pentaerythritol diacrylate 85.6% (target product), pentaerythritol ...

Embodiment 3

[0021] Put 1411g (90%) of dipentaerythritol and 5644g of dimethylformamide into the reactor with reflux water separator, heat to reflux at 155°C, wait until dipentaerythritol reaches the dissolution equilibrium, add 1800g of acrylic acid, sulfo-functionalized all-silicon medium Porous molecular sieve 109g, p-hydroxyanisole 27.2g, butyl ether 1000g. Reflux dehydration and esterification reaction at 95°C for 7.5 hours, and 435 g of water was separated. Stop heating and reflux, and cool down to 50°C. Filtration and recovery of the sulfo-functionalized all-silicon mesoporous molecular sieve catalyst. Under the condition of vigorous stirring, gradually add saturated sodium carbonate solution to the filtrate to make the material pH=8, separate the water layer, and then wash the organic layer with distilled water three times to make the material neutral. Finally, the solvent was removed under reduced pressure and filtered (0.6MPa) to obtain 2165g of a light yellow, transparent visc...

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PUM

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Abstract

The invention belongs to the field of crylic acid ester synthesis, and in particular discloses a preparation method of a high-purity (bi)pentaerythritol crylic acid non-complete esterification product. The defects in the prior art that the non-complete esterification rate of (bi)pentaerythritol and crylic acid is low and the purity is low are overcome. The preparation method comprises the following steps of: firstly, mixing a solvent with (bi)pentaerythritol, carrying out heating reflux so as to completely or partially dissolve the (bi)pentaerythritol, when the dissolution is balanced, sequentially adding the crylic acid, a catalyst, a polymerization inhibitor and a water-carrying agent, carrying out backflow esterification reaction; when the reaction is accomplished, neutralizing, decolorating, removing the solvent and filtering so as to obtain the (bi)pentaerythritol crylic acid non-complete esterification product. By using appropriate solvents, the (bi)pentaerythritol is completely or partially dissolved so as to be subjected to esterification reaction with the crylic acid at average phases; and the generated non-complete esterification product is high in purity and good in use performance.

Description

technical field [0001] The invention belongs to the field of acrylate synthesis, in particular to a method for preparing high-purity incomplete esterification products of pentaerythritol or dipentaerythritol and acrylic acid. Background technique [0002] Both pentaerythritol acrylate and dipentaerythritol acrylate are important multifunctional polymerizable 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 perfor...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08
Inventor 单玉华常彬彬曹鹰高秋敏栾宁万宇司坤坤
Owner CHANGZHOU XIAOGUO INFORMATION SERVICES
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