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Method for preparing cylohexanediol diglycidyl ether

A technology of diglycidyl ether and cyclohexanediol, applied in the direction of organic chemistry, can solve the problems of deepening product color, strong corrosion of equipment, increasing energy consumption, etc., to achieve environmental protection, shorten process time, and save The effect of energy consumption

Active Publication Date: 2011-11-23
昌德新材科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this type of catalyst solves the disadvantages of strong water absorption, strong volatility, high toxicity, and strong corrosion to equipment of the boron trifluoride ether complex catalyst, and the perchlorate catalyst is also convenient to use, but because the catalyst is in a solid state Existence, is a heterogeneous reaction system, low catalytic activity, high reaction temperature, used to synthesize high boiling point 1,2-cyclohexanediol diglycidyl ether will not only increase energy consumption, but also deepen the color of the product, Reduce product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 1mol epoxycyclohexane, 30mol water, and 0.0002mol fluoroboric acid into the reaction kettle, react between 75°C and 85°C, react until the epoxycyclohexane is completely hydrated, add 3mol of toluene for dehydration, and dehydrate Keep warm at 70°C to 75°C, then add 0.003mol of fluoboric acid, dropwise add 2.5mol of epichlorohydrin, react at 70°C to 75°C for 4 to 6 hours, after the reaction is complete, add 2.55mol of NaOH solution dropwise, drop After the addition, keep it warm at 40°C to 50°C for 4 to 5 hours. After the reaction, separate the oil phase, wash the oil phase with water until neutral, then filter and distill off the light components to obtain the product.

Embodiment 2

[0015] Take 1.5mol of water and 0.01mol of fluoboric acid into the reaction kettle, keep the reaction kettle between 10°C and 20°C and add 1mol of epoxycyclohexane dropwise, and continue the reaction until the epoxycyclohexane is completely hydrated , add 1.5mol of cyclohexane for distillation and dehydration, keep warm at 10°C to 20°C after dehydration, add 2.1mol of epichlorohydrin dropwise, react at 10°C to 20°C for 9 to 10 hours, the reaction is complete, Add 4.15mol Na dropwise 2 CO 3 After the solution is added dropwise, keep it warm at 30°C to 40°C and react for 5 to 6 hours. After the reaction, separate the oil phase, wash the oil phase with water until it is neutral, then filter and distill off the light components to obtain the product.

Embodiment 3

[0017] Take 15mol of water and 0.003mol of fluoroboric acid into the reaction kettle, keep the reaction kettle between 40°C and 50°C and add 1mol of epoxycyclohexane dropwise, after the dropwise addition, continue to react until the epoxycyclohexane is completely hydrated, Add 1.5mol of toluene for distillation and dehydration. After dehydration, continue to keep warm at 50°C-60°C, add 1.8mol of epichlorohydrin dropwise, and react at 50°C-60°C for 4-5 hours. After the reaction is complete, add dropwise 1.85mol NaOH solution, after the dropwise addition, keep it warm at 50°C to 60°C and react for 3 to 4 hours. After the reaction, separate the oil phase, wash the oil phase with water until it is neutral, then filter and distill off the light components to obtain the product.

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PUM

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Abstract

The invention discloses a method for preparing cylohexanediol diglycidyl ether. The method comprises: generating cyclohexanediol through the hydration of cyclohexene oxide; synthesizing o-chlorohydrin ether through the ring-opening reaction of dehydrated cyclohexanediol and epichlorohydrin; reacting the o-chlorohydrin ether and alkali to synthesize 1,2-cylohexanediol diglycidyl ether crude products; and obtaining products by performing oil-water separation, washing and filtration on the crude products and distilling out light components, wherein catalysts for both hydration and ring-opening reaction are fluoboric acid, and the mol ratio of cyclohexene oxide to water to fluoboric acid to epichlorohydrin is 1:5-50:0.002-0.1:1.8-2.5. The method has the advantages of taking fluoboric acid as the catalysts for both hydration and ring-opening reaction, realizing the organic unity of the catalysts in a two-step process, reducing energy consumption, shortening process time, avoiding large amounts of waste water produced by repeated recrystallization during the purification of cyclohexanediol and helping to environmental protection.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanediol diglycidyl ether. Background technique [0002] 1,2-Cyclohexanediol diglycidyl ether is an epoxy additive with excellent performance. The common method is to hydrate epoxycyclohexane under the action of a hydration catalyst to generate crude 1,2-cyclohexanediol product, and then remove the color and impurities of the crude 1,2-cyclohexanediol product through repeated recrystallization; Then use 1,2-cyclohexanediol product and epichlorohydrin to synthesize chlorohydrin ether under the action of ring-opening catalyst; finally, react chlorohydrin ether with alkali to synthesize 1,2-cyclohexanediol diglycidol Ether crude product, wash the crude product to neutrality, filter and distill off the light component to obtain the product. [0003] The hydration catalysts used in the above process are usually sulfuric acid, sulfonic acid, acidic resin, etc. Such oxoacids generally have strong oxidiz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/27C07D301/00
Inventor 屈铠甲夏立锋何双林蒋卫和陈旭辉
Owner 昌德新材科技股份有限公司
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