Preparation method of diallyl-terminated polyether and diallyl-terminated polyether

A bisallyl-capped and polyether technology is applied in the field of preparation of bisallyl-terminated polyether and bisallyl-terminated polyether, which can solve the problem of low molecular weight, unfavorable sealant application and widening of molecular weight distribution. and other problems to achieve the effect of high product purity

Active Publication Date: 2022-03-11
WUHAN OXIRAN SPECIALTY CHEM CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Limited by the current synthesis technology of allyl alcohol polyether, the synthesized molecular weight is low, and after capping, the molecular weight of the product will double, and the molecular weight distribution will widen, which is not conducive to the subsequent application of sealants

Method used

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  • Preparation method of diallyl-terminated polyether and diallyl-terminated polyether
  • Preparation method of diallyl-terminated polyether and diallyl-terminated polyether
  • Preparation method of diallyl-terminated polyether and diallyl-terminated polyether

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preparation example Construction

[0034] see figure 1 , a method for preparing a high molecular weight diallyl-terminated polyether provided in an embodiment of the present invention, comprising the following steps:

[0035] Step S1: providing a difunctional polyoxypropylene ether and an alkoxide reagent, the difunctional polyoxypropylene ether having two hydroxyl groups.

[0036] The molecular formula of the difunctional polyoxypropylene ether is:

[0037]

[0038] Wherein, n is a natural number, and the molecular weight of the difunctional polyoxypropylene ether is 4000-20000.

[0039] The difunctional polyoxypropylene ether is a polyoxypropylene ether having two functional groups capable of participating in the subsequent alkoxide reaction, that is, the two hydroxyl functional groups in the above molecular formula. That is, the difunctional polyoxypropylene ether is polyether diol.

[0040] The alkoxide reagent includes at least one of potassium tert-butoxide, sodium hydride, potassium methylate and p...

Embodiment 1

[0066] Add 1000 g of difunctional polyoxypropylene ether with a molecular weight of 4000 into a reaction kettle with a volume of 2 L, and add 22 g of sodium hydride with a mass fraction of 60% as an alkoxide reagent.

[0067] After sealing the reactor and replacing it with nitrogen for 3 times, pre-react the polyether diol and sodium hydride at room temperature for 30 minutes; then slowly raise the temperature to 130°C, stir together during the heating process, and maintain the reaction pressure at 0.01MPa -0.1MPa, in order to remove the gas generated during the reaction, the reaction time of alkoxide is 6h.

[0068] Lower the temperature of the polyether polyol salt formed after the alkoxide reaction to 30°C-40°C, add 42.1g of propylene chloride, increase the pressure in the reactor to 300kPa, and raise the temperature in the reactor to 60°C- After reacting for 6 hours at 70°C, a turbid light yellow reaction intermediate was obtained.

[0069] Add 22g of phosphoric acid with...

Embodiment 2

[0071] The difference from Example 1 is: the molecular weight of polyether polyol is 8000, the mass of sodium hydride is 11g; the mass of allyl chloride is 21g; the mass of phosphoric acid is 11g.

[0072] Other steps are the same as those in Embodiment 1, and will not be repeated here.

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Abstract

A method for preparing a bisallyl-terminated polyether, comprising the steps of: providing a difunctional polyoxypropylene ether and an alkoxide reagent, the bifunctional polyoxypropylene ether having two hydroxyl groups; mixing the difunctional polyoxypropylene ether The functional polyoxypropylene ether and the alkoxide reagent are subjected to an alkoxide reaction to obtain an alkoxide compound; ether. The invention also provides a bisallyl-terminated polyether. The bisallyl-terminated polyether prepared by the method for preparing the bisallyl-terminated polyether provided by the invention has a large molecular weight and a narrow molecular weight distribution.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a preparation method of a diallyl-terminated polyether and a diallyl-terminated polyether. Background technique [0002] The middle part of the molecular chain of bisallyl-terminated polyether is polyoxypropylene ether, and the two ends of the molecular chain are allyl groups. It has the following general formula: [0003] [0004] where n is a natural number. [0005] Since both ends of the diallyl-terminated polyether molecule have highly reactive allyl groups, as a chemical intermediate, it is an ideal crosslinking agent for polymerization reactions, especially in the field of silicones, through which diallyl The C=C double bond of the group-terminated polyether reacts with the Si-H of the hydrogen-containing silicone oil to prepare the grafted silicone oil. In addition, the bisallyl-terminated polyether molecule has polyether as the main chain and the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/338C08G65/337C08G65/328
CPCC08G65/338C08G65/337C08G65/328
Inventor 王辉任凡王亮张静付艳梅胡哲付远波刘敏耿聪江晨浩
Owner WUHAN OXIRAN SPECIALTY CHEM CO
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