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Preparation method of diallyl terminated polyether

A bisallyl-capped and polyether technology is applied in the field of preparation of bisallyl-terminated polyethers, which can solve the problems of high viscosity of intermediate products and low end-capping rate, and achieve complete alkoxide exchange and end-capping. High rate, simple and easy-to-control process

Pending Publication Date: 2022-06-24
江苏瑞洋安泰新材料科技有限公司 +1
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Problems solved by technology

[0006] Therefore, it is necessary to develop a method for the preparation of diallyl-terminated polyether to solve the problems of excessive viscosity and low end-capping rate of intermediate products in the reaction process.

Method used

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  • Preparation method of diallyl terminated polyether
  • Preparation method of diallyl terminated polyether
  • Preparation method of diallyl terminated polyether

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preparation example Construction

[0031] According to a typical embodiment of the present invention, there is provided a preparation method of bisallyl-terminated polyether, such as figure 1 As shown, the method includes:

[0032] Step S1, performing the following operations into the polyether: adding an alkoxide reagent to the polyether to carry out the alkoxide reaction, and then removing the generated alcohol in a vacuum; then adding chloropropene to carry out the end-capping reaction; wherein, the first step is to carry out the alkoxide reaction. During the above operation, the molar mass ratio of the alkoxide reagent to the hydroxyl group in the polyether is 1: (0.1-0.5);

[0033] In the above technical scheme, when controlling the operation for the first time, the ratio of the molar mass of the alkoxide reagent to the hydroxyl group in the polyether is 1: (0.1-0.5), which is beneficial to complete the alkoxide and control the reaction system. If the ratio is too small (that is, the addition of alkoxide ...

Embodiment 1

[0046] Embodiment 1, a kind of preparation method of bisallyl-terminated polyether

[0047]In the following 2L reaction kettle, add 1000 grams of poly(1,2-propylene glycol) with a molecular weight of 4000, 13.5 grams (0.25mol) of solid sodium methoxide, raise the temperature to 60 degrees, and remove methanol in vacuum (pressure is 10KPa~1KPa) , after 1 hour of reaction, the system viscosity is 25000mPa.s. Close the vacuum valve, add 19.1 g (0.25 mol) of allyl chloride, and react for 10 minutes. Then, 14.85 g (0.275 mol) of solid sodium methoxide was added, and the methanol was removed in vacuo (the pressure was 10 KPa-1 KPa). After 1 hour of reaction, the viscosity of the system was 26000 mPa.s. Close the vacuum valve, add 22.9 g (0.30 mol) of allyl chloride, and react for 10 minutes. Excessive allyl chloride is recovered by distillation. After cooling, the pH was adjusted to 6 with phosphoric acid, and the salt was removed by filtration to obtain an allyl-terminated polye...

Embodiment 2

[0048] Embodiment 2, a kind of preparation method of bisallyl-terminated polyether

[0049] In the following 2L reactor, add 1000 grams of poly(1,2-propylene glycol) with a molecular weight of 8000, 5.25 grams (0.075mol) of solid potassium methoxide, raise the temperature to 70 degrees, and remove methanol in vacuum (pressure is 10KPa~1KPa) , after 2 hours of reaction, the system viscosity is 32000mPa.s. The vacuum valve was closed, 5.74 g (0.075 mol) of allyl chloride was added, and the reaction was carried out for 30 minutes. Then, 5.25 g (0.075 mol) of solid potassium methoxide was added, and the methanol was removed in vacuo (the pressure was 10 KPa-1 KPa). After 2 hours of reaction, the viscosity of the system was 35000 mPa.s. The vacuum valve was closed, 5.74 g (0.075 mol) of allyl chloride was added, and the reaction was carried out for 30 minutes. 5.25 g (0.075 mol) of solid potassium methoxide was added, and methanol was removed in vacuo (the pressure was 10 KPa-1 K...

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Abstract

The invention discloses a preparation method of diallyl-terminated polyether, which comprises the following steps: adding an alkalization reagent into polyether to carry out alkalization reaction, and then removing generated alcohol in vacuum; then adding chloropropene to carry out an end capping reaction; repeating the operation for more than or equal to one time; wherein when the operation is carried out for the first time, the molar mass ratio of the alkoxide reagent to hydroxyl in the polyether is 1: (0.1-0.5); in all the operations, the ratio of the total molar amount of the alkoxide reagent to the molar weight of hydroxyl in the polyether is (1.0-1.2): 1, and the ratio of the total molar amount of the chloropropene to the molar weight of hydroxyl in the polyether is (1.1-1.5): 1; and carrying out post-treatment on the product to obtain the allyl-terminated polyether. The method solves the problem that the high viscosity of polyether alkoxide is not beneficial to continuous reaction with an alkoxide reagent, the viscosity of a reaction system is greatly reduced, and the end capping rate of allyl polyether is improved.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of a bisallyl-terminated polyether. Background technique [0002] Diallyl-terminated polyether is a special type of polyether in which both ends of the polyether are end-capped by allyl groups. Among them, α,ω-diallyl poly(1,2-propylene glycol) (as shown in the figure below) is a special class of bisallyl-terminated polyethers, which are mainly used in the preparation of alkoxysilane-terminated polyethers. [0003] [0004] The method for preparing this polyether is generally Williams ether condensation method, which can be divided into one-step method and two-step method according to process conditions. In the one-step process, the polyether, alkoxide reagent and allyl chloride end-capping agent are simultaneously added to the reaction system for direct reaction. The method is simple to operate, the crude product is directly obtained after the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337C08G65/331
CPCC08G65/337C08G65/3312
Inventor 唐红定张旭建黄兵
Owner 江苏瑞洋安泰新材料科技有限公司
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