Synthetic method for crosslinking agent-pentaerythritol allyl ether for high molecular polymerization

A technology of pentaerythritol allyl ether and polymer polymerization, applied in ether preparation, organic chemistry and other directions, can solve the problems of poor selectivity, dark product color, low yield of polyol ether, etc., to improve the reaction selectivity and yield Effect

Active Publication Date: 2008-08-13
NANJING WELL CHEM
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Problems solved by technology

[0003] The above synthesis method is because the alkalinity in the reaction system is too strong, so the yield of the polyol ether of the halogenated olefin obtained by synthesis is low, the product color is deep, the by-product is many, the selectivity is poor, and the allyl group suitable for polymerization cannot be obtained. Polyol Ether

Method used

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  • Synthetic method for crosslinking agent-pentaerythritol allyl ether for high molecular polymerization
  • Synthetic method for crosslinking agent-pentaerythritol allyl ether for high molecular polymerization

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Experimental program
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Embodiment 1

[0021] Embodiment 1: Add 800g pentaerythritol, 700g sodium hydroxide, 1353g allyl chloride, 450gPEG800, 700g distilled water in 5L, 316L stainless steel reactor, pressurize to 0.2MPa with nitrogen, check airtightness, heating starts Stir, stir and react at a temperature of 60-120°C for 8-10 hours, take samples and analyze the materials in the kettle, after the etherification reaction is completed, discharge the materials while they are hot, separate the sodium chloride from the reaction mixture by centrifugation, and pour the filtrate into the liquid separation tank, and add an equal volume of tap water, and add metered 20% hydrochloric acid aqueous solution to neutralize, the pH value is about 7, then static layering, the lower water layer is separated, the upper oil phase is returned to the reactor, and the vacuum is 20mmHg , dehydration under reduced pressure at a temperature of 100°C to 120°C, removal of trace by-products of propylene alcohol and low molecular weight substa...

Embodiment 2

[0023] In reactor, add 800g pentaerythritol, 982g potassium hydroxide, 1353g allyl chloride, 450gPEG800, 982g distilled water, the condition and operation of synthetic pentaerythritol allyl ether are the same as embodiment 1, filter to obtain refining pentaerythritol allyl ether mixture 1100g, The yield is 81.3% (based on the amount of allyl chloride charged), and its mass composition is 10% pentaerythritol allyl disubstituted; trisubstituted 72%; tetrasubstituted 18% through gas chromatographic analysis.

Embodiment 3

[0025] Add 800g pentaerythritol, 700g sodium hydroxide, 1353g allyl chloride, 200g tetrabutylammonium bromide, 700g distilled water in the reaction kettle, the condition and operation of synthetic pentaerythritol allyl ether are the same as embodiment 1, filter to obtain refined pentaerythritol propane Allyl ether mixture 1070g, yield is 79.1% (in terms of allyl chloride charging amount), through gas chromatography analysis and identification, its mass composition is pentaerythritol allyl ether disubstituted 7%; Three substituted 70%; Four substituted twenty three%.

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Abstract

The process of synthesizing pentaerythritol allyl ether as cross-linking agent for polymerization includes the following steps: mixing allyl chloride, alkali catalyst and pentaerythritol in the molar ratio of 3.0-5.5 to 3.0-5.5 to 1.0; etherification reaction at 60-80 deg.c for 8-10 hr under the action of phase transfer catalyst; neutralizing, water washing, desalting and filtering, degassing and refining. The phase transfer catalyst is one of ammonium tetrabutyl bromide and PEG200-PEG1000; and the alkali catalyst is sodium or potassium hydroxide in the concentration preferably of 30 %-50 %. The synthesis process has effectively raised reaction selectivity and produce yield, and the yield may reach 88 % accounting in allyl chloride.

Description

technical field [0001] The invention belongs to the technical field of halogenated olefin etherification of polyols, and relates to a synthesis method of pentaerythritol allyl ether, a crosslinking agent for polymer polymerization. Background technique [0002] Polyol allyl ether is a cross-linking agent widely used in polymer polymerization, and is widely used in the fields of pharmaceutical polymers, cosmetic polymers and emulsion polymers. At present, the synthetic methods for preparing such crosslinking agents are limited to the traditional Williamson (Cheng Liamson) method of halogenated olefins, and this method has attracted the attention of many researchers. Known Williamson (Williamson) method discloses in Japanese Patent Publication No. 48-22198, No. 54-32598, U.S. Patent No. 3312460 and German Patent No. 1021346, using sodium methylate, sodium metal, sodium hydroxide or hydroxide Aqueous or alcoholic solutions of potassium are used as alkali metallating reagents. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/06C07C43/178C07C41/01
Inventor 严军表余清彭文勇周霞娟
Owner NANJING WELL CHEM
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