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Clean production method of 1, 4-butanediol diglycidyl ether

A technology of diglycidyl ether and its production method, which is applied in the direction of organic chemistry, can solve the problem of excessive waste water, and achieve the effects of less waste water, simple operation, and reasonable design of the preparation process

Inactive Publication Date: 2020-10-09
江苏三木化工股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the existing synthetic method has a high yield, it produces more waste water, so it is urgent to develop a green and environmentally friendly 1,4-butanediol diol that produces less waste water in the production process, has mild conditions, is easy to operate, and is suitable for industrial production. The preparation method of glycidyl ether

Method used

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  • Clean production method of 1, 4-butanediol diglycidyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation method of 1,4-butanediol diglycidyl ether, it comprises the following steps:

[0025] (1) Add 200g of 1,4-butanediol and 1.4g of boron trifluoride-diethyl ether into a 2000ml four-neck flask, add 472.8g of epichlorohydrin dropwise at 70°C under stirring, add dropwise for 3 hours, and keep for 1 Hour;

[0026] (2) Then add 700g of toluene, heat up to 40°C, add 204.4g of solid NaOH, take 4 hours, keep for 1 hour, after the reaction is completed, transfer to a Buchner funnel for suction filtration, add a certain amount of phosphoric acid to the filtrate for neutralization , and then transferred to a separatory funnel for liquid separation. After the liquid separation, the toluene solvent was removed to obtain 484 g of 1,4-butanediol diglycidyl ether, with a yield of 99.5%.

Embodiment 2

[0028] A kind of preparation method of 1,4-butanediol diglycidyl ether, it comprises the following steps:

[0029] (1) Add 200g of 1,4-butanediol and 1.4g of perchloric acid to a 2000ml four-neck flask, add 472.8g of epichlorohydrin dropwise at 70°C under stirring, add dropwise for 3 hours, and keep for 1 hour (after testing Pre-reaction residual epichlorohydrin is more);

[0030] (2) Then add 700g of toluene, the temperature rises to 40°C, add 204.4g of solid NaOH, add for 4 hours, keep for 1 hour after the reaction is completed, transfer to a Buchner funnel for suction filtration, add a certain amount of phosphoric acid to the filtrate for neutralization, and then transfer Separation was carried out in a separating funnel, and the toluene solvent was removed after separation to obtain 390 g of 1,4-butanediol diglycidyl ether, with a yield of 80.2%.

Embodiment 3

[0032] A kind of preparation method of 1,4-butanediol diglycidyl ether, it comprises the following steps:

[0033] (1) Add 200g of 1,4-butanediol and 1.4g of boron trifluoride-ether to a 2000ml four-neck flask, add 472.8g of epichlorohydrin dropwise at 60°C under stirring, add dropwise for 3 hours, and keep for 1 hour ;

[0034] (2) Add 500g toluene, the temperature rises to 40°C, solid NaOH 204.4g, add for 4 hours, keep for 1 hour after the reaction is completed, transfer to the Buchner funnel for suction filtration, add a certain amount of phosphoric acid to the filtrate for neutralization, and then transfer to Separation was carried out in a separatory funnel, and the toluene solvent was removed after separation to obtain 475 g of 1,4-butanediol diglycidyl ether with a yield of 97.7%.

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Abstract

The invention discloses a clean production method of 1, 4-butanediol diglycidyl ether. The method comprises the following steps: generating chlorohydrin ether from 1, 4-butanediol and epoxy chloropropane under the action of a catalyst, and carrying out ring-closure reaction under the action of alkali to generate 1, 4-butanediol diglycidyl ether. The optimal synthetic route is obtained by screeningthrough a large number of experiments, the raw material conversion rate is high, the yield can reach over 99%, generated wastewater is little, conditions are mild, operation is easy and convenient, and the method is suitable for clean industrial production.

Description

technical field [0001] The invention relates to a clean production method of 1,4-butanediol diglycidyl ether, which belongs to the technical field of polymer materials. Background technique [0002] 1,4-Butanediol diglycidyl ether is an important organic chemical intermediate, which is widely used in the coating industry and synthetic chemical industry. It can be used as an epoxy reactive diluent, which is a multifunctional reactive diluent with flexibility Good quality, low viscosity, low volatility, low odor, low toxicity, etc. It is used as a diluent for epoxy resin to reduce the viscosity of the epoxy system and improve the mechanical properties of the epoxy cured product. Although the existing synthetic method has a high yield, it produces more waste water, so it is urgent to develop a green and environmentally friendly 1,4-butanediol diol that produces less waste water in the production process, has mild conditions, is easy to operate, and is suitable for industrial pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/28C07D303/27
CPCC07D301/28C07D303/27
Inventor 殷杰
Owner 江苏三木化工股份有限公司
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