Preparation method of 1, 4-butanediol diglycidyl ether

A technology of diglycidyl ether and butanediol, which is applied in ether preparation, alkylene oxide preparation ether, organic chemistry and other directions, can solve the problem of high hydrolysis chlorine, achieve low hydrolysis chlorine, reduce TOC, and solve the effect of high organic content

Pending Publication Date: 2022-01-28
JIANGSU KUMHO YANGNONG CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrolysis chlorine of the 1,4-butanediol diglycidyl ether prepared by the above synthetic method is still relatively high

Method used

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  • Preparation method of 1, 4-butanediol diglycidyl ether
  • Preparation method of 1, 4-butanediol diglycidyl ether
  • Preparation method of 1, 4-butanediol diglycidyl ether

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preparation example Construction

[0025] The invention provides a kind of preparation method of 1,4-butanediol diglycidyl ether, comprising the following steps:

[0026] Mix 1,4-butanediol, Lewis acid catalyst, epichlorohydrin and a water-immiscible solvent for etherification and ring-opening reaction to obtain chlorohydrin ether;

[0027] Mix the chlorohydrin ether with a water-immiscible solvent, add a main reaction catalyst, and dropwise add an aqueous alkali solution to carry out negative pressure closed-loop reflux dehydration to obtain 1,4-butanediol diglycidyl ether;

[0028] In the step-by-step dropwise addition of alkali aqueous solution to carry out negative-pressure closed-loop reflux dehydration, after each stage of dropwise addition of alkali aqueous solution, a section of negative-pressure closed-loop reflux dehydration is performed.

[0029] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art...

Embodiment 1

[0049] Add 160g of 1,4-butanediol, 160g of toluene and 2.5g of tin tetrachloride into a 2L reaction flask and stir evenly. After the temperature rises to 60°C, add 380g of epichlorohydrin dropwise for 2 hours. , heat up to 70°C and keep the ring-opening reaction for 4 hours to obtain a chlorohydrin ether solution; add 480g toluene and 0.8g polyethylene glycol 400 to the chlorohydrin ether solution, cool down to 42°C and add 85g dropwise at a uniform speed for the first time to a concentration of 50wt % NaOH solution, the first drop time is 0.5h, under the conditions of 42°C and 10Torr, the first negative pressure closed-loop reflux dehydration is 0.5h, and then the second dropwise addition of 85g of NaOH solution with a concentration of 50wt% under the condition of 42°C , the second dropping time is 1h, under the condition of 42°C and 10Torr, the second negative pressure closed-loop reflux dehydration is 0.5h, under the condition of 42°C, 85g of NaOH solution with a concentrati...

Embodiment 2

[0051] Add 160g of 1,4-butanediol, 480g of toluene and 2.5g of boron trifluoride into a 2L reaction flask and stir evenly. After the temperature rises to 60°C, add 380g of epichlorohydrin dropwise for 1 hour. , heat up to 70°C and keep the ring-opening reaction for 5 hours to obtain a chlorohydrin ether solution; add 160g of toluene and 1.6g of polyethylene glycol 400 to the chlorohydrin ether solution, cool down to 42°C and then add 90g dropwise at a uniform speed for the first time to a concentration of 50wt % NaOH solution, the first drop time is 0.5h, under the condition of 42°C and 10Torr, the first negative pressure closed-loop reflux dehydration is 0.5h, and then the second dropwise addition of 90g of NaOH solution with a concentration of 50wt% under the condition of 42°C , the second dropping time is 1h, under the condition of 42°C and 10Torr, the second negative pressure closed-loop reflux dehydration is 0.5h, and the third dropwise adding 90g of NaOH solution with a c...

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Abstract

The invention provides a preparation method of 1, 4-butanediol diglycidyl ether, and relates to the technical field of organic synthesis. According to the invention, an efficient Lewis acid catalyst is adopted in an etherification reaction stage of 1, 4-butanediol and epoxy chloropropane, then a catalyst is added through a main reaction, an aqueous alkali solution is dropwise added in a segmented mode, and negative-pressure closed-loop reflux dehydration is conducted in a segmented mode, so that the water content of a reaction system is reduced, the reaction forward process is promoted, the prepared 1, 4-butanediol diglycidyl ether product is low in hydrolytic chlorine and high in yield, the residual alkali amount and TOC of wastewater are reduced, the problems of too high residual alkali amount and high organic matter content in saline water are solved, and industrial clean production of the 1, 4-butanediol diglycidyl ether is realized; and the preparation method has the advantages of stable process, continuous production operation, avoidance of tedious solid caustic soda feeding, high safety, low raw material consumption and low production cost.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 1,4-butanediol diglycidyl ether. 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. [0003] At present, the synthesis of 1,4-butanediol diglycidyl ether mostly uses 1,4-butanediol as a raw material, and under the action of a catalyst (such as Lewis acid or tetrabutylammonium bromide), it is separated from epichlorohydrin. Ring, ring-closing reaction with base in two steps. The ring-open...

Claims

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Application Information

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IPC IPC(8): C07D301/26C07D301/32C07D303/30C07C41/03C07C43/13
CPCC07C41/03C07D301/26C07D301/32C07D303/30C07C43/137
Inventor 侯晶晶孙祥杨颖陈铭铸刘华朱毓新奚羽俞孝伟
Owner JIANGSU KUMHO YANGNONG CHEM CO LTD
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