Preparation method of trimethylolpropane diallyl ether

Abstract

The invention discloses a preparation method of trimethylolpropane diallyl ether. A reaction process comprises the steps of: firstly, carrying out azeotropic dehydration on trimethylolpropane and alkali metal hydroxide in the presence of butyl ether to obtain trimethylolpropane alkali metal salt, then subjecting chloropropene and the trimethylolpropane alkali metal salt to etherification reaction, removing peroxide from a reaction fluid after the etherification reaction, and carrying out vacuum distillation to obtain the trimethylolpropane diallyl ether. In the invention, solid sodium hydroxide or potassium hydroxide is used as a reaction raw material to reduce side reactions; nitrogen protection and a phase transfer catalyst are not used so that the cost is saved; the butyl ether is used as a reaction medium and an azeotropic dehydrating agent so that the content of the trimethylolpropane diallyl ether is greatly improved and the content of triether and monoether is reduced; the product is stable and reliable in quality, the production operation is simple and convenient and is easy to apply, three wastes are less, and the preparation process is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing trimethylolpropane diallyl ether, in particular to a method for preparing trimethylolpropane diallyl ether without using a catalyst. Background technique [0002] Trimethylolpropane diallyl ether (TMPDE), as a resin air-drying agent, has many special and excellent properties, and is widely used in the fields of unsaturated resins and alkyd resins to improve their drying and water resistance. No need to add wax to polish. The preparation method of trimethylolpropane diallyl ether (TMPDE) has been reported at home and abroad, such as Chinese patents CN1431184A, CN1301687A, CN1082020A, Japanese patents JP60231625A, JP60252440A, U.S. patent US3355502A, etc., trimethylolpropane di The preparation method of allyl ether (TMPDE) is generally obtained by etherification reaction using trimethylolpropane, alkali metal hydroxide and allyl chloride as raw materials. The reaction generally uses excess alkali and allyl...

AI Technical Summary

Problems solved by technology

The preparation method of trimethylolpropane diallyl ether (TMPDE) has been reported at home and abroad, such as Chinese patents CN1431184A, CN1301687A, CN1082020A, Japanese patents JP60231625A, JP60252440A, U.S. patent US3355502A, etc., trimethylolpropane di The preparation method of allyl ether (TMPDE) is generally obtained by etherification reaction using trimethylolpropane, alkali metal hydroxide and allyl chloride as raw materials. The reaction generally uses excess alkali and allyl chloride. An aqueous solution with a concentration of 40-50% is used, but the water content in the reaction system is too high, which makes chloropropene easy to hydrolyze to generate allyl alcohol, which increases the occurrence of side reactions. During the reaction, mainly use toxic benzene solvents, or use active Larger, ketone and ester solvents that easily cause side reactions, and the use of expensive and unrecoverable phase transfer catalysts increase product costs, and the obtained trimethylolpropane diallyl ether (TMPDE) product The content of monoether and triether is high, especially the content of triether is high, the product quality is poor and unstable, which is not conducive to the final use of the product

The process of the above method is complicated, the equipment investment is large, the requirements are high, the product yield is low, and the production cost is high, which is not conducive to industrial production