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Polyarylether-polysiloxane copolymer and preparation method thereof

A technology of polysiloxane and polyarylether, applied in the field of polyarylether-polysiloxane copolymer and its preparation, can solve the problem of poor oil resistance and solvent resistance, limit the application range of copolymers, reduce the mechanical strength of materials, etc. problems, to achieve the effect of improving mechanical strength, improving physical and chemical properties and processing performance, and the preparation method is mature and simple

Active Publication Date: 2018-05-22
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to obtain good mechanical strength, the ABA type tri-block copolymer must have a higher number average molecular weight (usually above 60,000), but this severely limits the relative content of A and B components, because some If the length of the chain segment is too long, it will cause phase separation beyond the necessary limit, which will seriously reduce the mechanical strength of the material.
while (AB) n Type block copolymers are not subject to this restriction, and can flexibly adjust the relative content and relative chain length of the two components according to actual application requirements, so they have many performance advantages. However, due to the limitations of PPO structure and copolymer synthesis method, long-term lag in its research
In addition, due to the poor oil resistance and solvent resistance of PPO and PDMS, and the pure PDMS segment will crystallize at around -50°C, this greatly limits the application range of copolymers.

Method used

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  • Polyarylether-polysiloxane copolymer and preparation method thereof
  • Polyarylether-polysiloxane copolymer and preparation method thereof
  • Polyarylether-polysiloxane copolymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0106] In a 1L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, add M n Be 5600 PPO-2OH (1a) 5.6g (1mmol), B (C 6 f 5 ) 3 56mg and 300mL of chlorobenzene, stirred and heated to 70°C. Add M to the constant pressure dropping funnel n 11g (1mmol) of PS-2H(2e) at 11000, and then added dropwise to the flask in 12 times (each interval 0.5h, each time about 1mL). As the reaction progressed, it was observed that bubbles escaped slowly from the solution, and the viscosity of the reaction system gradually increased. Continue to react for 3 hours after the dropwise addition, the viscosity of the reaction system has not increased significantly, and there is no gas escape, stop the reaction, cool to room temperature, precipitate the reaction mixture into 1000mL methanol, filter out the white rubber-like product, and vacuum at 80°C Dry to constant weight, the resulting (AB) n The yield of type polyarylether-polysiloxane copol...

Embodiment 2

[0108] In a 1L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, add M n 4400 PPO-2OH (1d) 4.4g (1mmol), B (C 6 f 5 ) 3 22mg and 265mL of chlorobenzene, stirred and heated to 80°C. Add M to the constant pressure dropping funnel n 7700 PS-2H (2d) 7.7g (1mmol), and then added dropwise to the flask 5 times (every interval of 1h, each time about 1.5mL). As the reaction progressed, it was observed that bubbles escaped slowly from the solution, and the viscosity of the reaction system gradually increased. Continue to react for 4 hours after the dropwise addition, the viscosity of the reaction system has not increased significantly, and there is no gas escape, stop the reaction, cool to room temperature, precipitate the reaction mixture into 1000mL methanol, filter out the white blocky product, and vacuum at 100°C Dry to constant weight. Earned (AB) n The yield of type polyarylether-polysiloxane copolymer is 98.2%, M ...

Embodiment 3

[0110] Add M n 8300 PPO-2OH (1e) 8.3g (1mmol), B (C 6 f 5 ) 3 17mg and 232mL of chlorobenzene, stirred and heated to 120°C. Add M to the constant pressure dropping funnel n 19g (1mmol) of PS-2H(2k) at 19000 was added dropwise into the flask in 20 times (20min interval between each time, about 1mL each time). After the dropwise addition, the reaction was continued for 1 h, then the reaction was stopped, cooled to room temperature, the reaction mixture was precipitated into 1000 mL of methanol, the white rubbery product was filtered out, and vacuum-dried at 120°C to constant weight. Earned (AB) n The yield of type polyarylether-polysiloxane copolymer is 98.2%, M n : 168800, PDI: 3.45.

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Abstract

The invention relates to the technical field of organosilicone industry, and provides a polyarylether-polysiloxane copolymer and a preparation method thereof in order to overcome defects of the priorart. By taking phenolic hydroxyl group terminated polyarylether and hydrogen terminated polysiloxane as raw materials and by utilizing a catalytic dehydrogenation and polycondensation method, an Si-Hbond at the tail end of a polysiloxane molecular chain is activated through a catalyst, so that the two raw materials are in dehydrogenation coupling reaction, an (AB)n type multi-block copolymer of which the structure is regular is formed through polycondensation, and soft / hard segments are connected together through an Si-O-Ph bond; an obtained (AB)n type polyarylether-polysiloxane multi-block copolymer has good mechanical performance, good heat resistance and good oil and solvent resistance.

Description

technical field [0001] The invention relates to the technical field of organic silicon industry, in particular to a polyarylether-polysiloxane copolymer and a preparation method thereof. Background technique [0002] Polysiloxane materials have many unique and excellent properties, so they have been widely used in many fields of the national economy, and have become an indispensable class of important polymer materials in modern society. However, due to the high flexibility of polysiloxane molecular chains (especially polydimethylsiloxane PDMS), it is necessary to add a vulcanizing agent for vulcanization in practical applications, so that crosslinking reactions occur between polysiloxane molecular chains, forming Rubber with three-dimensional network structure, in addition, fillers (such as gas phase SiO 2 etc.) for reinforcement to improve its mechanical strength and expand its application range. [0003] Around the 1970s, with the in-depth research on the synthesis meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C08L83/12C08L71/12C08L69/00C08L81/06
CPCC08G77/46C08L69/00C08L71/123C08L81/06C08L83/12C08L2201/08
Inventor 胡应乾张方耿梦鸾张鹏胡承刚邬继荣
Owner HANGZHOU NORMAL UNIVERSITY
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