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Low-hydrolyzed-chlorine 1,4-butanediol diglycidyl ether production method

A technology of diglycidyl ether and production method, which is applied in the direction of organic chemistry, can solve the problems of large amount of wastewater, high cost, and high hydrolyzed chlorine, and achieve the effects of reducing wastewater discharge, low production cost, and reduced hydrolyzed chlorine

Active Publication Date: 2017-08-01
HUBEI GREENHOME MATERIALS TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a production method of low-hydrolyzed chlorine 1,4-butanediol diglycidyl ether, to solve the existing technical problems of high hydrolyzed chlorine, large amount of waste water, and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 39.6Kg alcohol, 88Kg toluene, 0.15Kg boron trifluoride, 0.6Kg tin tetrachloride into a 500L reactor, heat up, when the temperature reaches 65°C, add 92.4Kg epichlorohydrin dropwise, and control the temperature at 65~ 70°C, after about 2 hours of dripping, continue to keep warm for 3 hours; cool down to 20°C, add 57.4Kg of 48% liquid caustic soda dropwise, finish adding 15 minutes, the temperature of the closed-loop reaction is 45°C, keep warm for 1h, turn on the circulating hot water, and increase the reaction Temperature to 70°C, keep warm for 3.5h; stand still, drain salt water, wash with water, and the upper oil phase is rectified to obtain 88.4Kg of 1,4-butanediol diglycidyl ether, the epoxy value is 0.7880 eq / 100Kg, hydrolysis Chlorine 225 ppm.

Embodiment 2

[0020] Add 40.5Kg alcohol, 90Kg toluene, 0.15Kg boron trifluoride, 0.6Kg tin tetrachloride to a 500L reactor, raise the temperature, when the temperature reaches 65°C, add 105Kg epichlorohydrin dropwise, and control the temperature at 65-70 ℃, drop for about 2 hours, continue to keep warm for 3 hours; cool down to 20 ℃, add 77.6Kg of 48% liquid caustic soda dropwise, after 15 minutes, the temperature of the closed-loop reaction is 45 ℃, keep warm for 1 hour, turn on the circulating hot water, and increase the reaction temperature To 70 ℃, keep warm for 3.5h; stand still, drain the salt water, wash with water, and the upper oil phase is rectified to obtain 98.5Kg of 1,4-butanediol diglycidyl ether, the epoxy value is 0.7773 eq / 100Kg, and the hydrolyzed chlorine 223 ppm.

Embodiment 3

[0022] Add 40.5Kg alcohol, 90Kg toluene, 0.15Kg boron trifluoride, 0.6Kg tin tetrachloride to a 500L reactor, raise the temperature, when the temperature reaches 65°C, add 105Kg epichlorohydrin dropwise, and control the temperature at 65-70 ℃, drop for about 2 hours, continue to keep warm for 3 hours; cool down to 20 ℃, add 73.8Kg of 48% liquid caustic soda dropwise, after 15 minutes, the temperature of the closed-loop reaction is 45 ℃, keep warm for 1 hour, turn on the circulating hot water, and increase the reaction temperature to 70°C, keep warm for 3.5 hours; let it stand, drain the brine, wash with water, and the upper oil phase is rectified to obtain 98 Kg of 1,4-butanediol diglycidyl ether, the epoxy value is 0.7590 eq / 100Kg, and the hydrolyzed chlorine 225 ppm.

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Abstract

The invention discloses a low-hydrolyzed-chlorine 1,4-butanediol diglycidyl ether production method. The method is characterized by comprising the following specific steps of performing ring-opening reaction, performing ring-closure reaction, draining saline water and washing, rectifying an upper-layer oil phase to obtain 1,4-butanediol diglycidyl ether, dehydrating through a desolvent to obtain a finished product of the low-hydrolyzed-chlorine 1,4-butanediol diglycidyl ether. The production method disclosed by the invention has the advantages of high product quality, low production cost, high efficiency in a production process, environmental friendliness, small emission and the like. In ring-closure reaction of the production method disclosed by the invention, a method of adopting low temperature at first and then high temperature is utilized; hydrolyzed chlorine of the prepared 1,4-butanediol diglycidyl ether is 200 to 300ppm, the hydrolyzed chlorine is obviously reduced, quality is remarkably improved, alkali liquid using amount is greatly reduced at the same time, and wastewater discharge in a reaction process is reduced.

Description

technical field [0001] The invention relates to a production method of low-hydrolyzed chlorine 1,4-butanediol diglycidyl ether. The method can further reduce the hydrolyzed chlorine of a diluent, improve product quality, reduce the amount of waste water in industrial production, and save production costs. Background technique [0002] 1,4-Butanediol diglycidyl ether is a long-chain difunctional epoxy reactive diluent, usually used as a toughening diluent for epoxy resin, widely used in epoxy systems such as solvent-free coatings, laminations, and adhesives . The active epoxy group contained in the diluent participates in the curing reaction, and no volatile matter is generated, which effectively improves the operating environment and product performance, and in addition to diluting, it can also increase the flexibility of the cured product. Composite materials such as wind turbine blades are widely used. [0003] Hydrolyzed chlorine is a very important characteristic index...

Claims

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Application Information

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IPC IPC(8): C07D301/00C07D303/24
CPCC07D301/00C07D303/24
Inventor 余永登孙亮
Owner HUBEI GREENHOME MATERIALS TECH INC
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