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Method for synthesizing pentaerythritol tetraglycidyl ether

A technology of glycidyl ether and pentaerythritol tetraglycidyl ether, which is applied in the field of synthesis of pentaerythritol tetraglycidyl ether, can solve the problems of incomplete reaction, uncontrollable reaction, low yield, etc., to increase yield, reduce product color and hydrolyze chlorine, The effect of promoting a complete response

Inactive Publication Date: 2020-05-05
ANHUI XINYUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the problem that the reaction existing in the prior art is difficult to control, the reaction is incomplete, and the yield is on the low side

Method used

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  • Method for synthesizing pentaerythritol tetraglycidyl ether
  • Method for synthesizing pentaerythritol tetraglycidyl ether
  • Method for synthesizing pentaerythritol tetraglycidyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Weigh 34g (0.25mol) of pentaerythritol and put it into a four-neck flask with stirring, add 102g of dioxane, heat up while stirring, and add a composite catalyst (boron trifluoride etherate complex and tetrachloromethane) to 90-95°C Tin) were 0.60g and 1.50g respectively, and 115.6g (1.25mol) of epichlorohydrin was added dropwise, and kept for 2h after dripping for 4h. The above solution was put into a distillation flask to remove the solvent, the temperature was controlled below 110°C, the holding time was 30min, and the vacuum degree was kept above 0.095MPa. Add 252 g of toluene to the intermediate after solvent removal, keep stirring, add 0.60 g of benzyltriethylammonium bromide to it after raising the temperature to 40-45 ° C, and add 22.5 g of solid alkali sodium hydroxide (0.563 mol) within 2 hours , added in four times with an interval of 30 minutes; then the temperature was raised to 60-65° C., 70.3 g (0.563 mol) of 32% liquid caustic soda was dripped within 1 h...

Embodiment 2

[0022] Weigh 34g (0.25mol) of pentaerythritol and put it into a four-neck flask with stirring, add 102g of dioxane, heat up while stirring, and add a composite catalyst (boron trifluoride etherate complex and tetrachloromethane) to 90-95°C Tin) were 0.41g and 1.03g, respectively, 69.4g (0.75mol) of epichlorohydrin was added dropwise, and the temperature was kept for 2h after 4h. The above solution was put into a distillation flask to remove the solvent, the temperature was controlled below 110°C, the holding time was 30min, and the vacuum degree was kept above 0.095MPa. Add 252g of chloroform to the intermediate after solvent removal, stir continuously, add 0.41g of benzyltriethylammonium bromide to it after heating up to 40-45°C, and add 12.5g (0.31mol) of solid alkali sodium hydroxide within 2h , added in four times with an interval of 30 minutes; then the temperature was raised to 60-65°C, and 39.1 g (0.31 mol) of liquid caustic soda was dripped within 1 hour and kept for 2...

Embodiment 3

[0024] Weigh 34g (0.25mol) of pentaerythritol and put it into a four-necked flask with stirring, add 102g of chloroform, raise the temperature while stirring, and raise the temperature to 90-95°C, add 1.31g of catalyst boron trifluoride, and dropwise add 185.0g of epichlorohydrin (2.0mol), after 4 hours of dripping, keep warm for 2 hours. The above solution was put into a distillation flask to remove the solvent, the temperature was controlled below 100°C, the holding time was 30min, and the vacuum degree was kept above 0.095MPa. Add 252 g of ethylene dichloride to the intermediate after solvent removal, stir continuously, add 0.88 g of benzyltriethylammonium bromide to it after raising the temperature to 40-45 ° C, and add 37.5 g of solid alkali sodium hydroxide within 2 hours ( 0.94mol), added in four times with an interval of 30min; then the temperature was raised to 60-65°C, 117.2g (0.94mol) of liquid caustic soda was dripped within 1h and kept for 2h. After the reaction ...

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Abstract

The invention relates to a method for synthesizing pentaerythritol tetraglycidyl ether, which comprises the following steps: (1) a ring opening reaction: pentaerythritol and epoxy chloropropane are adopted as raw materials to synthesize an intermediate product chlorohydrin ether, wherein one or more of a boron trifluoride diethyl ether complex, stannic chloride, fluoboric acid, boron trifluoride and zinc perchlorate are used as catalysts, the reaction temperature is 40-100 DEG C, and the feeding ratio of the mole number of pentaerythritol hydroxyl to epoxy chloropropane is 1: 3.0 to 1: 8.0, and the solvent is one or more of methylbenzene, cyclohexane, dichloroethane, chloroform and dioxane; (2) solvent removal: the solvent is removed from the product obtained by the ring-opening reaction to obtain a chlorohydrin ether intermediate; (3) ring-closure reaction: a certain amount of solvent is added into the chlorohydrin ether intermediate, and then ring-closure reaction with alkali is carried out; and (4) post-treatment: the crude product after the ring-closure reaction is washed with tap water for multiple times, and the washed crude product is distilled in a distillation still. The method has the advantages of good reaction control and high product yield, and the product is mainly used as an acidic resin cross-linking agent and a diluent for perfusion and packaging.

Description

technical field [0001] The invention relates to a synthesis method of pentaerythritol tetraglycidyl ether. Background technique [0002] Pentaerythritol tetraglycidyl ether is a widely used diluent. The molecular structure contains four epoxy groups, so it has high reactivity and can increase the crosslinking density with other groups. The product is mainly used to prepare various epoxy resin castables, solvent-free coatings, dipping glue, dripping glue and adhesives. [0003] At present, there are the following three methods for synthesizing pentaerythritol tetraglycidyl ether at home and abroad. The quality of the products obtained by the first two methods is very good, but their synthetic raw materials are relatively expensive, the process is complex and there are big problems in safety. Therefore, a third method, a two-step synthesis, was adopted. Compared with the previous two methods, this method not only has easy-to-obtain raw materials, but also has a reasonable p...

Claims

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Application Information

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IPC IPC(8): C07D301/26C07D303/30
CPCC07D301/26C07D303/30
Inventor 程振朔赵普杰陈海军孙其飞黄健
Owner ANHUI XINYUAN CHEM
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