Method for preparing pentaerythrite allyl ether

Abstract

The present invention pertains to the technical field of organic synthesis, providing a method to prepare allyl pentaerythritol ether compound mainly composed of allyl pentaerythritol ether. The preparation method includes the following steps: (1) pentaerythritol, alkali metal hydroxide, water and inert organic solvent are mixed according to a proper ratio, heated and agitated during reaction; (2) a proper dosage of phase-transfer catalyst is added into the reactant mixture, allyl halide is added slowly and supplementary phase-transfer catalyst is added when the allyl halide is added, and then the mixture is agitated to end the etherification reaction; (3) after reaction, the salt, the unreacted alkali-metal hydroxide and the phase-transfer catalyst in the system are removed by water, the separated organic layer is distilled under normal pressure to remove the light component, and the desired product is achieved by vacuum distillation. The preparation method has the advantages of high yield of target products, low production cost, simple operation process, high security, and industrial production can be realized easily.

Description

technical field [0001] The invention relates to a preparation method of pentaerythritol allyl ether, in particular to a preparation method of a pentaerythritol triallyl ether mixture. Background technique [0002] Due to the active groups such as ether groups, ethylenic bonds and hydroxyl groups, allyl pentaerythritol ether is often used as a chain extender for super absorbent resins, thickeners, unsaturated polyesters, polyurethane resins, epoxy resins , UV curing resin and other polymer synthesis, while making the polymer self-drying. Pentaerythritol triallyl ether mixtures that are commonly used in industry are pentaerythritol triallyl ether-based mixtures, and the most commonly used mixtures are those in which the mass percentage of pentaerythritol triallyl ether is between 70% and 90%. [0003] U.S. Patent No. 3,428,693 discloses a method for preparing pentaerythritol allyl ether mixtures, using pentaerythritol, dipentaerythritol, and allyl chloride as raw materials, u...

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Problems solved by technology

[0003] U.S. Patent No. 3,428,693 discloses a method for preparing pentaerythritol allyl ether mixtures, using pentaerythritol, dipentaerythritol, and allyl chloride as raw materials, using sodium oxide as a catalyst, and using a large amount of dimethyl sulfoxide as a solvent to obtain mainly pentaerythritol tetra Allyl ether, dipentaerythritol tetraallyl ether, dipentaerythritol pentaallyl ether, and dipentaerythritol hexaallyl ether, etc., are difficult to post-process due to the use of a large amount of organic solvents

[0004] Chinese patent CN96115830.1 discloses a preparation method of polyol allyl ether, but this method is mainly aimed at the trimethylolpropane system, using a pressurized device for reaction, and has the disadvantages of large equipment investment and low reaction conversion rate. , not suitable for industrial production of pentaerythritol allyl ether

[0005] The Japanese patent application whose publication number is JP63162640 discloses a preparation method of pentaerythritol allyl ether. Pentaerythritol, alkali metal hydroxide and chloropropene are used as reaction raw materials, catalyzed by a phase transfer catalyst, and alkali metal hydroxide is added at intervals in batches. The aqueous solution of the compound and allyl chloride, the reaction is carried out at normal temperature and pressure, but because the sodium salt of pentaerythritol is not fully contacted with allyl chloride, the product yield is low

[0006] Publication number is that the Japanese patent application of JP63162641 discloses a kind of preparation method of pentaerythritol allyl ether, is reaction raw material by pentaerythritol, alkali metal hydroxide and chloropropene, uses the alkali metal salt of tertiary amine and halogen as joint catalyst, because Tertiary amines are toxic, which poses a safety hazard in the production process

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