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A multiple functional group (methyl) acrylate synthesis and purification method

A technology of acrylates and purification methods, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as low product yield and purity, emulsification, and poor product color

Active Publication Date: 2007-08-22
SHANGHAI HUAYI NEW MATERIAL
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Problems solved by technology

[0004] The purpose of the present invention is exactly in order to avoid the reaction system sticking to the wall due to the use of a single entrainer cyclohexane in the method reported by the existing patent, the chroma of the final product is not good due to the use of solid adsorption decolorization, and the emulsification phenomenon occurs during post-treatment. The yield and purity of the product are relatively low, and then a method for the synthesis and purification of a high-purity multifunctional group (meth)acrylate developed

Method used

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Experimental program
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Effect test

Embodiment 1-7

[0009] In the 500ml flask, add (meth)acrylic acid, polyhydric alcohol, entrainer and be equivalent to the copper acetate polymerization inhibitor of reaction solution 0.5~0.8% (quality) and the p-toluenesulfonic acid catalyst of 2.0~3.0% (quality), Heating with silicone oil, the temperature of the oil bath is controlled within the range of 112-114°C, and the reaction temperature is controlled between 60-90°C. The water in the reaction process is continuously taken out of the system by the entrainer through the water separator. The reaction was confirmed to be complete when the generated water reached a near theoretical value. When the temperature of the reaction solution drops to 50-55°C, wash with deionized water equivalent to 30% (volume) of the reaction solution, keep the temperature at 45-50°C, stir for 3 minutes, settle for 30 minutes, and divide the water; Wash the reaction solution twice with a concentration of 6% (mass) NaOH aqueous solution that is equivalent to 52% ...

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Abstract

The invention relates to a process for preparing multifunctional (methyl) acrylate, which can be widely applied in the fields of radiation solidified paint, printing ink, adhesive and polymer modification. The preparation comprises using mixed entrainer, subjecting the crude product to post-treatment and purification. The obtained product has a yield of greater than 95%, a purity above 99%, and a chromaticity (APHA) lower then 20.

Description

technical field [0001] The invention relates to a preparation method of a high-purity multifunctional group (meth)acrylate. Specifically, it is a method of using a mixed entrainer as a water-carrying agent in the esterification process and washing with a salt solution in the post-treatment process of the crude product, thereby improving the color of the product and increasing the ester content and yield. technical background [0002] At present, there are many methods for producing multifunctional (meth)acrylates, but the most important method is still the direct esterification method. The direct esterification process is simple, the reaction time is short, the temperature is low, and it is easy to be adopted by people. But this method also faces many difficult problems that need to be solved urgently: 1) the color of the product is poor, 2) the post-treatment of the reaction solution is difficult and easy to emulsify, 3) the purity and yield of the product are low. People...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/54C07C67/08
Inventor 马建学张庆怀刘书举袁海英
Owner SHANGHAI HUAYI NEW MATERIAL
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