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Method for preparing alkoxylated polyol acrylate

A technology of neopentyl glycol diacrylate and acrylic acid, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of explosion hazard, low product yield, and easy pollution of wastewater environment , to achieve the effect of improving product quality and high product yield

Active Publication Date: 2015-02-11
内蒙古宏远天呈科技发展有限公司
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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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of propoxylated (2) neopentyl glycol diacrylate (PO2-NPGDA), comprising the steps of:

[0028] 1) Put 80g of propoxylated (2) neopentyl glycol, 57.6g of acrylic acid, 4.5g of solid acid catalyst, and 0.5g of phenothiazine into a 500ml three-necked flask, start stirring, and stir for 2 hours to carry out Esterification reaction.

[0029] 2) Turn on the vacuum pump, control the pressure in the reaction flask to 0.05Mpa, and then increase the temperature in the flask to 120°C to generate reflux, and continuously flow out the water generated 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 was lowered to normal temperature.

[0030] 3) Filter the material, distill off residual acrylic acid and water under the conditions of temperature 98°C and vacuum degree 0.09Mpa. When the acid value is controlled at 0....

Embodiment 2

[0032] A preparation method of ethoxylated (4) bisphenol A diacrylate (EO4-BPADA), comprising the steps of:

[0033] 1) Put 100g of ethoxylated (4) bisphenol A, 39.2g of acrylic acid, 4.5g of solid acid catalyst, and 0.5g of p-hydroxyanisole into a 500ml three-necked flask, start stirring, and stir for 2 hours to carry out Esterification reaction.

[0034] 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 generate reflux, and continuously flow out the water generated by the reaction through the water separator. The reaction time is 3.5 hours, and the reaction is detected The acid value of the solution was 35 mgKOH / g, and the heating was stopped. Start cooling down to room temperature.

[0035] 3) Filter the material, distill off residual acrylic acid and water under the conditions of temperature 105°C and vacuum degree 0.095Mpa. When the acid value is controlled at 0.76mgKOH / g, the d...

Embodiment 3

[0037] A preparation method of ethoxylated (3) trimethylolpropane triacrylate (EO3-TMPTA), comprising the steps of:

[0038] 1) Put 80g of ethoxylated (3) trimethylolpropane, 71.5g of acrylic acid, 4.5g of solid acid catalyst, and 0.5g of p-hydroxyanisole into a 500ml three-necked flask, start stirring, and stir for reaction 2 hours, the esterification reaction was carried out.

[0039] 2) Turn on the vacuum pump, control the pressure in the reaction flask to 0.098Mpa, and then increase the temperature in the flask to 98°C to generate reflux, and continuously flow out the water generated by the reaction through the water separator. The reaction time is 2 hours, and the reaction is detected The acid value of the solution was 35 mgKOH / g, and the heating was stopped. Start cooling down to room temperature.

[0040] 3) Filter the material, distill off the residual acrylic acid and water under the conditions of temperature 115°C and vacuum degree 0.098Mpa. When the acid value is ...

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Abstract

The invention relates to a method for preparing alkoxylated polyol acrylate. The method comprises the following steps of adding main materials, namely alkoxylated polyol and acrylic acid, into an esterification reaction vessel, adding a solid acid catalyst, adding a polymerization inhibitor, reacting under the conditions of certain temperature and vacuum degree, removing the solid acid catalyst through filtering, and removing the remaining acrylic acid and water through distillation, thereby obtaining the alkoxylated polyol acrylate. The method has the beneficial effects that the product does not contain volatile organic substances and is environmental-friendly and green, the product yield is high, no environmental pollution is caused, and the quality of the product is improved.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to a method for preparing an alkoxylated polyol acrylate, which can be used as a radiation curing reactive diluent. Background technique [0002] The synthesis methods of acrylate reactive diluent mainly include direct esterification method, transesterification method, acid chloride method and addition esterification method. The water generated during the synthesis process is removed by dehydrating agent. Commonly used dehydrating agents include benzene, Toluene, xylene, cyclohexane, etc., are carried away by forming an azeotropic liquid with the water produced in 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 high boiling point; the use of benzene series solvents has been restricted in industries such as coatings, inks, and adhesives. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/54C07C67/08
Inventor 黄凤岐庞震杨树峰李锴
Owner 内蒙古宏远天呈科技发展有限公司