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A side-chain hydrogen-containing silyne hybrid high temperature resistant polymer and its preparation method

A technology of high temperature-resistant polymer and hydrogen-containing silicon, which is applied in the field of organic polymer materials, can solve the problems of limited development space and application scope of materials, poor molding and processing performance, and high curing temperature, so as to improve molding processing performance and high temperature resistance. , The effect of improving heat resistance and reducing curing temperature

Active Publication Date: 2020-05-08
FUJIAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, these silyne hybrid polymers have defects such as less active groups that can participate in the curing reaction, higher curing temperature, and poor molding and processing performance in the structure, which limits the development space and application range of this type of material.

Method used

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  • A side-chain hydrogen-containing silyne hybrid high temperature resistant polymer and its preparation method
  • A side-chain hydrogen-containing silyne hybrid high temperature resistant polymer and its preparation method
  • A side-chain hydrogen-containing silyne hybrid high temperature resistant polymer and its preparation method

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preparation example Construction

[0024] A method for preparing a side-chain hydrogen-containing silane hybrid high-temperature-resistant polymer, characterized in that it comprises the following steps:

[0025] Step 1: Under the protection of an inert gas, react trichlorethylene with butyl lithium to synthesize ethynyl dilithium;

[0026]

[0027] Step 2: Under the protection of an inert gas, react dichlorosilane with the ethynyl dilithium synthesized in step 1 to synthesize ethynyl-silane;

[0028]

[0029] Where: R 1 , R 2 is phenyl or vinyl;

[0030] Step 3: Under the protection of an inert gas, react trifluoromethanesulfonic acid with the ethynyl-silane synthesized in step 2 to obtain trifluoromethanesulfonated ethynyl-silane with activated side chain;

[0031]

[0032] where R 1 , R 2 is phenyl or vinyl; any integer of x≥0, any integer of y>0;

[0033] Step 4: Under the protection of an inert gas, react sodium borohydride with the trifluoromethanesulfonated ethynyl-silane generated in step...

Embodiment 1

[0047] Prepare a kind of side chain hydrosilyne hybrid high temperature resistant polymer (wherein, R 1 , R 2 Both are vinyl; x=0)

[0048] Under the protection of high-purity nitrogen, add 16.7mL of butyllithium, 10mL of tetrahydrofuran and 10mL of anhydrous ether into a four-necked flask, control the temperature of the system at -20 to -40°C, and drop 1.2mL of trichlorohydrin through a constant pressure dropping funnel. Ethylene, after the dropwise addition, the system was kept at this temperature for 2 hours. Then, the temperature was controlled at -20 to -40° C., and a solution of 1.9 mL of divinyldichlorosilane and 10 mL of tetrahydrofuran was added dropwise. After the dropwise addition, the system was kept at this temperature for 2 hours. Then control the temperature at -10 to -40°C, continue to slowly add a solution of 2.4mL trifluoromethanesulfonic acid and 20mL tetrahydrofuran dropwise, keep the system at this temperature for 3 hours after the dropwise addition, and...

Embodiment 2

[0052] Prepare a kind of side chain hydrosilyne hybrid high temperature resistant polymer (wherein, R 1 , R 2 Both are phenyl groups; x=0)

[0053] Under the protection of high-purity nitrogen, add 16.7mL of butyllithium, 10mL of tetrahydrofuran and 10mL of anhydrous ether into a four-necked flask, control the temperature of the system at -20 to -40°C, and drop 1.2mL of trichlorohydrin through a constant pressure dropping funnel. Ethylene, after the dropwise addition, the system was kept at this temperature for 2 hours. Then, the temperature was controlled at -20 to -40°C, and a solution of 2.8 mL of diphenyldichlorosilane and 10 mL of tetrahydrofuran was added dropwise. After the dropwise addition, the system was kept at this temperature for 3 hours. Then control the temperature at -10 to -40°C, continue to slowly add a solution of 2.4mL trifluoromethanesulfonic acid and 20mL tetrahydrofuran dropwise, keep the system at this temperature for 3 hours after the dropwise additi...

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Abstract

The invention provides a silicon-alkyne hybrid high-temperature-resistant polymer containing hydrogen on a side chain. The structural general formula of the polymer is shown in structural formula 1, wherein x is any integer greater than or equal to zero, and y is any integer greater than zero; R1 is phenyl or vinyl; and R2 is phenyl or vinyl. The invention also provides a preparation method of the polymer. The preparation method comprises the following steps: 1. reacting trichloroethylene with butyl lithium to synthesize dilithium acetylide; 2. reacting dichlorosilane with the dilithium acetylide to synthesize ethynyl-silane; 3. reacting trifluoromethane sulfonic acid with the ethynyl-silane to obtain trifluoromethane sulfonated ethynyl-silane with an activated side chain; and 4. reacting sodium borohydride with the trifluoromethane sulfonated ethynyl-silane, wherein the steps 1-4 are all carried out in an inert gas protective atmosphere. According to the invention, the polymer can be crosslinked and cured at a low temperature, and has favorable molding processability and heat resistance; and the preparation method has the advantages that the process is simple, the conditions are easy to control and the operation convenience is high.

Description

technical field [0001] The invention relates to the technical field of organic polymer materials, in particular to a side-chain hydrogen-containing silyne hybrid high-temperature-resistant polymer and a preparation method thereof. Background technique [0002] With the in-depth application of high-temperature resistant materials in high-tech fields such as aerospace, electronic appliances and power energy, higher requirements are put forward for their performance. All kinds of high-strength, high-modulus, high-temperature resistance and oxidation resistance have excellent comprehensive performance High-performance materials for long-term use in complex environments have emerged. Among them, introducing appropriate inorganic elements (such as Si, B, N, etc.) The prepared polymer contains inorganic elements and organic groups in the main chain or side chain of the structure. It is a type of organic-inorganic hybrid material with excellent properties of both organic materials ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 陈明锋刘玉惠范先谋刘灿培
Owner FUJIAN NORMAL UNIV
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