Method for preparing pentaerythrite allyl ether

A technology of pentaerythritol allyl ether and pentaerythritol, which is applied in the field of preparation of pentaerythritol allyl ether, can solve the problems of difficult post-processing, large investment in equipment, insufficient contact, etc., and achieves easy industrial production, simple operation process, and suppression of side effects. The effect of the reaction

Inactive Publication Date: 2008-06-18
ZHUHAI FEIYANG NOVEL MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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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

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  • Method for preparing pentaerythrite allyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Raw materials and dosage:

[0030] Monopentaerythritol (>98%) 150g

[0031] Sodium hydroxide (99%) 150g

[0032] water 150g

[0033] Xylene 40g

[0034] Allyl chloride 281g (about 300ml)

[0035] Tetrabutylammonium bromide 4.5g

[0036] In a four-necked flask equipped with a reflux condenser, a stirrer, a thermometer and a dropping funnel, put monopentaerythritol, sodium hydroxide, water and xylene respectively, heat and stir to raise the temperature to 110°C. Start to add 1.5g of tetrabutylammonium bromide, and start to add 100ml of allyl chloride dropwise, control the drop rate slowly, and the dropwise addition is completed in about 1.5 hours; the reflux may be relatively large during the dropwise addition, and the temperature will drop to 90°C for a while, drop Halfway through, 1.0 g of tetrabutylammonium bromide was added. Pay attention to the continuous water separation when adding dropwise. After the dropwise addition of 100 ml of allyl chloride was complet...

Embodiment 2

[0038] Raw materials and dosage:

[0039] Monopentaerythritol (>98%) 150g

[0040] Sodium hydroxide (99%) 150g

[0041] water 150g

[0042] Xylene 40g

[0043] Allyl chloride 281g (about 300ml)

[0044] Benzyltriethylammonium chloride 4.5g

[0045]Process and equipment are with embodiment 1. Final product: 179g of product was obtained by distillation, wherein the content of diether was 4.09%, the content of triether was 81.4%, the content of tetraether was 14.51%, and the molar yield was 63.4% based on pentaerythritol.

Embodiment 3

[0047] Raw materials and dosage:

[0048] Monopentaerythritol (>98%) 300kg

[0049] Sodium hydroxide (99%) 300kg

[0050] Water 600kg

[0051] Tetrabutylammonium bromide 13kg

[0052] Xylene 80kg

[0053] Allyl chloride 600kg

[0054] It is carried out in a pilot test kettle equipped with a reflux condenser (condensed with an ice machine), a heating mantle, a thermometer, an agitator, a manhole, and a feeding port. Clean the reaction kettle to check whether the equipment is in good condition, turn on the ice machine, and pour 300kg of monopentaerythritol, 300kg of sodium hydroxide, 200kg of water, 80kg of xylene, and 5kg of tetrabutylammonium bromide according to the formula. After feeding the material, cover the manhole cover, raise the temperature, and stir in a jog. After the stirring is in normal operation, stir the material evenly. When the temperature of the kettle rose to about 110°C, the allyl chloride was slowly added dropwise. Depending on the temperature of t...

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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...

Claims

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Application Information

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IPC IPC(8): C07C43/178C07C41/01
Inventor 肖阳肖增钧李凡锋徐叶辉
Owner ZHUHAI FEIYANG NOVEL MATERIALS
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