Process for preparing polyalcohol acrylate

A technology of alcohol acrylate and acrylic acid, applied in the field of compound synthesis, can solve the problems of intractability, large amount, unfavorable environmental protection and the like

Active Publication Date: 2005-11-09
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method will produce a large amount of waste water containing salt and organic matter in the process of neutralization and washing; this kind of waste water is difficult to treat and is unfavorable to environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation of embodiment 1. pentaerythritol triacrylate

[0016] Add 100g pentaerythritol, 175g acrylic acid, 200g toluene, 7g p-toluenesulfonic acid, 0.6g p-tert-butylcatechol, 0.3g phenothiazine, 1g of activated carbon, heat up until the system is in a reflux state, toluene and water are azeotroped, and the water generated by the reaction is continuously taken out of the system through the water separator until no more water comes out and the temperature of the reaction solution is stable, which can be regarded as an esterification reaction At the end point, the temperature of the reaction system during the entire esterification reaction is 103-115° C., and the acid value of the reaction system is about 30-40 mgKOH / g. Lower the temperature to 70-80°C, add 80g of 1# solid base to the reaction solution, raise the temperature again to keep the system in reflux state for 1-1.5 hours, and a small amount of water generated can be azeotroped out of the system with tolue...

Embodiment 2

[0017] Embodiment 2. Preparation of propoxylated glycerol triacrylate

[0018] Add 150g of propoxylated glycerin, 128g of acrylic acid, 166.8g of benzene, 11g of p-toluenesulfonic acid, 0.34g of p-tert-butylcatechol, 0.17g of phenothiazine, and 1.4g of activated carbon in the same reaction flask as in Example 1 , followed by the same esterification reaction as in Example 1. The temperature of the reaction system during the entire esterification reaction is 85-104°C. What added in the neutralization process was 80g2# solid alkali, and the subsequent vacuum debenzene process was identical to the process of removing toluene in Example 1. The acid value of the obtained propoxylated glycerin triacrylate is ≤0.1mgKOH / g, and the hue is ≤40APHA. During the neutralization process, 4.5 g of waste water was produced.

Embodiment 3

[0019] Example 3. Preparation of Propoxylated Trimethylolpropane Triacrylate

[0020] Add 160g propoxylated trimethylolpropane, 118g acrylic acid, 222.4g cyclohexane, 7g p-toluenesulfonic acid, 0.4g2,6-di-tert-butyl p-cresol in the same reaction flask as in Example 1 , 0.2g phenothiazine, 0.6g gac, followed by the same esterification reaction as in Example 1. The temperature of the reaction system during the entire esterification reaction is 82-102°C. What added in the neutralization process was 80g3# solid alkali, and the subsequent vacuum decyclohexane process was the same as the embodiment to remove toluene process 1. The acid value of the obtained propoxylated trimethylolpropane triacrylate is ≤0.1mgKOH / g, and the hue is ≤40APHA. The neutralization process produced 4.5 g of waste water.

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Abstract

A process for preparing polyol acrylate used as the reactive diluent of irradiation solidification includes such steps as providing polyol and acrylic acid, mixing, adding solvent, polymerizing inhibitor, catalyst and decoloring agent, heating, reflux, adding solid alkali for neutralizing, filtering for removing solid, adding P-hydroxyphenyl mether, vacuum removal of solvent and filtering. Its advantage is no generation of sewage.

Description

technical field [0001] The invention relates to the field of compound synthesis; the final product-polyol acrylate can be used as a radiation curing reactive diluent. Background technique [0002] The preparation of polyol acrylate generally adopts the method of direct esterification of alkyd. A certain molar ratio of polyol and acrylic acid are reacted at a certain temperature in the presence of an acidic catalyst, a polymerization inhibitor and a solvent. During the reaction process, the water generated by the reaction is continuously taken out of the reaction system through the azeotropic solvent and water. After the esterification reaction is finished, the acidic catalyst and residual acrylic acid in the reaction system are removed by washing with neutralized water, and then the solvent is removed by vacuum to obtain the final product. This preparation method will produce a large amount of waste water containing salt and organic matter in the process of neutralization a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54
Inventor 黄凤岐王久河
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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