Synthesis of methacrylate allyl propyl ester

A technology of allyl methacrylate and methacrylic acid, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of difficult recovery of allyl alcohol, troublesome operation, and time-consuming, etc., and achieve The method is simple and easy, saves raw materials, and has the effect of simple operation

Inactive Publication Date: 2003-04-16
湖北武大有机硅新材料股份有限公司
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Problems solved by technology

The method is cumbersome to operate, time-consuming, and the yield is not high, and excessive allyl alcohol is difficult to recover
If the consumption of allyl alcohol is increased to 6 times that of methacrylic acid, the yield can be increased to 86% (Zhur. A large amount of allyl alcohol is difficult to recycle, which greatly increases the cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0017] The reaction was carried out in a three-necked flask equipped with a thermometer and a stirrer, the flask was connected with a fractionation column, the top of the fractionation column was connected with a water separator filled with benzene, and a reflux condenser was installed on the top of the water separator. Add 34.4 g (0.4 mol) of methacrylic acid, 92.9 g (1.6 mol) of allyl alcohol, 1 g of inhibitor hydroquinone, 4 g of catalyst p-toluenesulfonic acid, and 10 ml of benzene with water to the reaction flask, and heat to boiling and reflux , the temperature is 97-103 ℃, remove the water until the water is very slow, about 5-6 hours, and cool. The acid in the reaction mixture was neutralized with anhydrous sodium acetate until the pH of the solution was 6, filtered in a fume hood, the filtrate was rapidly distilled under reduced pressure with a water pump, the inorganic salt residue was discarded, 1 g of hydroquinone was added to the distillate, and 1 g of hydroquinone...

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Abstract

A process for synthesizing allyl methylacrylate includes such steps as under the existance of catalyst (p-toluenesulfonic acid) and polymerization inhibitor (hydroquinone), reaction between methylacrylic acid and allyl alcohol under the reflux condition while continuously removing the generated water, fractionating to recover the excessive allyl alcohol, and pressure-reduction distilling for purifying the product. Its advantages are high output rate (90-92%), high purity (98-99%), and no pollution.

Description

technical field [0001] The invention relates to the field of fine chemicals, and more particularly to a method for synthesizing allyl methacrylate. Background technique [0002] At present, there are three main methods for synthesizing allyl methacrylate, one is esterification, which is rarely reported in domestic literature. 3 times the amount of allyl alcohol was reacted with concentrated sulfuric acid as catalyst, hydroquinone as polymerization inhibitor, heated and refluxed for 6 hours, then steam distillation (about 2 hours), and the distillate was placed in a separatory funnel for The sodium carbonate solution and water were washed twice, dried for 24 hours, and distilled under reduced pressure, the yield was 76%. The method is troublesome and time-consuming to operate, the yield is not high, and the excess allyl alcohol is difficult to recover. If the amount of allyl alcohol is increased to 6 times that of methacrylic acid, the yield can be inc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54
Inventor 张治民刘秀英张彦谦廖俊陈圣云张先亮
Owner 湖北武大有机硅新材料股份有限公司
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