Method for preparing pentaerythritol triacrylate

A technology of pentaerythritol triacrylate and pentaerythritol, which is applied in the field of compound synthesis, can solve the problems of low product yield, explosion hazard, easy pollution of waste water environment, etc., achieve high product yield and improve product quality.

Active Publication Date: 2013-10-02
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] During the preparation process of acid chloride method, there are a large amount of HCL and SO 2 produced, it needs to be absorbed with lye and water, and its waste water is easy to cause pollution to the environment
[0005] In the process of synthesizing acrylate by addition esterification, it is required to directly react alcohol and acetylene under high temperature and pressure, especially acetylene has the risk of explosion and the product yield is low

Method used

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  • Method for preparing pentaerythritol triacrylate
  • Method for preparing pentaerythritol triacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of pentaerythritol triacrylate includes the following steps:

[0031] 1) Put 75g of pentaerythritol, 131g of acrylic acid, 4.5g of solid acid catalyst, and 0.5g of phenothiazine in a 500ml three-necked flask, turn on the stirring, stir and react for 2 hours to carry out the esterification reaction.

[0032] 2) Turn on the vacuum pump, control the pressure in the reaction flask to 0.05Mpa, then raise the temperature in the flask to 120°C to cause reflux, and continuously flow out the water produced by the reaction through the water separator. The reaction time is 5 hours, and the reaction is detected The acid value of the solution was 30 mgKOH / g, the temperature was stopped, and the temperature began to drop to room temperature.

[0033] 3) Filter the material, distill off the residual acrylic acid and water under the conditions of 98°C and 0.09Mpa vacuum. When the acid value is controlled at 0.92mgKOH / g, the distillation can be stopped and the temperature ...

Embodiment 2

[0035] A preparation method of pentaerythritol triacrylate includes the following steps:

[0036] 1) 75g of pentaerythritol, 131g of acrylic acid, 4.5g of solid acid catalyst, 0.5g of p-hydroxyanisole, placed in a 500ml three-necked flask, turned on the stirring, stirred and reacted for 2 hours to proceed the esterification reaction.

[0037] 2) Turn on the vacuum pump, control the pressure in the reaction flask to 0.075Mpa, and then increase the temperature in the flask to 110°C to cause reflux, and the water produced by the reaction will flow out continuously through the water trap. The reaction time is 3.5 hours, and the reaction is detected The acid value of the solution is 40 mgKOH / g, and the temperature rise is stopped. Start to cool down to room temperature.

[0038] 3) Filter the material, distill off the residual acrylic acid and water under the conditions of temperature 105℃ and vacuum degree of 0.095Mpa. When the acid value is controlled at 0.76mgKOH / g, the distillation c...

Embodiment 3

[0040] A preparation method of pentaerythritol triacrylate includes the following steps:

[0041] 1) Put 75g of pentaerythritol, 131g of acrylic acid, 4.5g of solid acid catalyst, and 0.5g of p-hydroxyanisole into a 500ml three-necked flask, turn on the stirring, stir and react for 2 hours to carry out the esterification reaction.

[0042] 2) Turn on the vacuum pump, control the pressure in the reaction flask to 0.098Mpa, then raise the temperature in the flask to 98°C to cause reflux, and continuously flow out the water produced by the reaction through the water separator. The reaction time is 2 hours, and the reaction is detected The acid value of the solution is 50 mgKOH / g, and the temperature rise is stopped. Start to cool down to room temperature.

[0043] 3) Filter the material, distill off the residual acrylic acid and water under the conditions of temperature 115℃ and vacuum degree 0.098Mpa. When the acid value is controlled at 0.58mgKOH / g, the distillation can be stopped an...

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Abstract

The invention relates to a method for preparing pentaerythritol triacrylate. The method comprises the following steps that pentaerythritol and acrylic acid are added into an esterification reaction container, then, solid acid catalysts are added, polymerization inhibitors are added, the reaction is carried out under the conditions of certain temperature and vacuum degree, then, solid acid catalysts are filtered out, the remained acrylic acid is removed through distillation, and the pentaerythritol triacrylate is obtained. Compared with the prior art, the method has the beneficial effects that volatile organic compounds are not contained, the product yield is high, the products are environment-friendly green products, no pollution is caused on the environment, and the quality of the products is improved.

Description

Technical field [0001] The invention relates to the field of compound synthesis, in particular to a method for preparing pentaerythritol triacrylate, which is suitable for radiation curing reactive diluents. Background technique [0002] The synthetic methods of acrylic active diluents mainly include direct esterification, transesterification, acid chloride and addition esterification. The water generated during the synthesis process is removed by dehydrating agents. Commonly used dehydrating agents include benzene, Toluene, xylene, cyclohexane, etc., are taken away by forming an azeotropic liquid with water produced by the esterification reaction. Alkanes are expensive and highly volatile; benzene has a low boiling point, high volatility, and toxicity; toluene is slightly less toxic than benzene; xylene has a higher boiling point; the use of benzene series solvents has been restricted in industries such as coatings, inks and adhesives. [0003] When preparing multifunctional acry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54
Inventor 黄健文黄凤岐许宝锁
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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