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Environment-friendly preparation method of polypropylene glycol diglycidyl ether

A technology of diglycidyl ether and polypropylene glycol, which is applied in organic chemistry and other fields, can solve the problems of cumbersome preparation methods, high cost, and excessive waste water, and achieve the effects of less waste water, simple operation, and mild conditions

Pending Publication Date: 2022-04-01
江苏三木化工股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the yields of the two methods are relatively high, 48% liquid caustic soda is used to react in method 1, and water is used for washing at the end of the reaction, and the waste water produced in the process is more, and water can take away part of the material in the washing process; while the method 2 Although the solid alkali method is adopted, it adopts a one-step method, in which the amount of solid alkali used is three times that of polyether, and both solid alkali and epichlorohydrin have serious excess problems, and epichlorohydrin needs to be recycled Utilization, the preparation method is more loaded down with trivial details, the cost is very high

Method used

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  • Environment-friendly preparation method of polypropylene glycol diglycidyl ether

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Effect test

Embodiment 1

[0024] A kind of environment-friendly preparation method of polypropylene glycol diglycidyl ether, it comprises the following steps:

[0025] (1) Add 400g polypropylene glycol 400 and 2.4g boron trifluoride-ether to a 2000ml four-neck flask, add 203.5g epichlorohydrin dropwise at 70°C under stirring, add dropwise for 4 hours, and keep for 2 hours;

[0026] (2), then add 600g of toluene, raise the temperature to 45°C, add 81.6g of solid NaOH, take 4 hours and keep for 2 hours;

[0027] (3) After the reaction, transfer to Buchner funnel for suction filtration, add a certain amount of glacial acetic acid to the filtrate for neutralization, then transfer to the separatory funnel for liquid separation, remove the toluene solvent after liquid separation to obtain polypropylene glycol dishrink 511 g of glyceryl ether, the yield is 97.6%.

Embodiment 2

[0029] A kind of environment-friendly preparation method of polypropylene glycol diglycidyl ether, it comprises the following steps:

[0030] (1) Add 400g polypropylene glycol 400 and 2.8g boron trifluoride-ether to a 2000ml four-neck flask, add 185g epichlorohydrin dropwise at 80°C under stirring, add dropwise for 4 hours, and keep for 2 hours;

[0031] (2), then add 800g of toluene, raise the temperature to 40°C, add 80g of solid NaOH, take 4 hours and keep for 2 hours;

[0032] (3) After the reaction, transfer to Buchner funnel for suction filtration, add a certain amount of glacial acetic acid to the filtrate for neutralization, then transfer to the separatory funnel for liquid separation, remove the toluene solvent after liquid separation to obtain polypropylene glycol dishrink Glyceryl ether 495g, the yield is 96.7%.

Embodiment 3

[0034] A kind of environment-friendly preparation method of polypropylene glycol diglycidyl ether, it comprises the following steps:

[0035] (1) Add 400g polypropylene glycol 400 and 3.2g boron trifluoride-ether to a 2000ml four-neck flask, add 203.5g epichlorohydrin dropwise at 70°C under stirring, add dropwise for 4 hours, and keep for 2 hours;

[0036] (2), then add 400g of toluene, heat up to 45°C, add 84g of solid NaOH, take 4 hours and keep for 2 hours;

[0037] (3) After the reaction, transfer to Buchner funnel for suction filtration, add a certain amount of glacial acetic acid to the filtrate for neutralization, then transfer to the separatory funnel for liquid separation, remove the toluene solvent after liquid separation to obtain polypropylene glycol dishrink 507g of glycerol ether, the yield is 96.9%.

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Abstract

The invention discloses an environment-friendly preparation method of polypropylene glycol diglycidyl ether, which comprises the following steps: generating chlorohydrin ether from polypropylene glycol 400 and epichlorohydrin under the action of a catalyst, and carrying out ring-closure reaction under the action of alkali to generate the polypropylene glycol diglycidyl ether. The optimal synthesis method is obtained through screening of a large number of experiments, the preparation method adopts a two-step method, solid alkali is used as a raw material in the second-step reaction to replace original liquid alkali, and glacial acetic acid is added into the final alkaline filtrate for neutralization, so that in the whole preparation process, less wastewater is generated, the condition is mild, the operation is simple and convenient, and the method is suitable for industrial production. The yield can reach 97.6%, and the method is a novel environment-friendly method for preparing the polypropylene glycol diglycidyl ether.

Description

technical field [0001] The invention relates to an environment-friendly preparation method of polypropylene glycol diglycidyl ether, which belongs to the technical field of polymer materials. Background technique [0002] Polypropylene glycol 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. This diluent is a difunctional reactive diluent with good flexibility, low viscosity, It has the characteristics of low volatility, low odor and low toxicity. It is used as a diluent for epoxy resin to reduce the viscosity of epoxy system, participate in the curing reaction of epoxy resin, and has high elasticity in molecular structure. Greatly improve its impact strength and thermal shock resistance, and improve the brittle defects of epoxy cured products. There are two existing synthesis methods: method 1: CN107629203A patent discloses a method for s...

Claims

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Application Information

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IPC IPC(8): C07D301/26C07D303/24
Inventor 殷杰惠正权
Owner 江苏三木化工股份有限公司
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