Silicon-alkyne hybrid high-temperature-resistant polymer containing hydrogen on side chain and preparation method thereof

A high-temperature-resistant polymer and hydrogen-containing silicon technology, applied in the field of organic polymer materials, can solve the problems of limited material development space and application range, poor molding and processing performance, and few active groups, so as to improve molding processing performance and durability High temperature capability, improvement of heat resistance, effect of lowering curing temperature

Active Publication Date: 2017-08-18
FUJIAN NORMAL UNIV
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  • Summary
  • 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 temper

Method used

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  • Silicon-alkyne hybrid high-temperature-resistant polymer containing hydrogen on side chain and preparation method thereof
  • Silicon-alkyne hybrid high-temperature-resistant polymer containing hydrogen on side chain and preparation method thereof
  • Silicon-alkyne hybrid high-temperature-resistant polymer containing hydrogen on side chain and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

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

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

[0026]

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

[0028]

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

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

[0031]

[0032] Where R 1 , R 2 Is phenyl or vinyl; any integer x≥0, y> Any integer of 0;

[0033] Step 4: Under the protection of inert gas, react sodium borohydride with the trifluoromethanesulfonated ethynyl-silane generated in step 3, and post-process to obtain th...

Example Embodiment

[0046] Example 1

[0047] Preparation of a side chain hydrogen-containing silylyne hybrid high temperature resistant polymer (wherein, R 1 , R 2 All are vinyl; x=0)

[0048] Under the protection of high-purity nitrogen, add 16.7mL butyllithium, 10mL tetrahydrofuran and 10mL anhydrous ether into a four-necked flask, control the temperature of the system at -20~-40℃, and add 1.2mL trichloride dropwise through a constant pressure dropping funnel. After the dropwise addition of ethylene is completed, the system is maintained to react at this temperature for 2 hours. Then, control the temperature at -20°C to -40°C, add dropwise a solution of 1.9 mL of divinyldichlorosilane and 10 mL of tetrahydrofuran, and maintain the system to react at this temperature for 2 hours after the addition is complete. Then control the temperature at -10~-40℃, continue to slowly drip the solution of 2.4mL trifluoromethanesulfonic acid and 20mL tetrahydrofuran. After the addition, maintain the system to reac...

Example Embodiment

[0051] Example 2

[0052] Preparation of a side chain hydrogen-containing silylyne hybrid high temperature resistant polymer (wherein, R 1 , R 2 All are phenyl; x=0)

[0053] Under the protection of high-purity nitrogen, add 16.7mL butyllithium, 10mL tetrahydrofuran and 10mL anhydrous ether into a four-necked flask, control the temperature of the system at -20~-40℃, and add 1.2mL trichloride dropwise through a constant pressure dropping funnel. After the dropwise addition of ethylene is completed, the system is maintained to react 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 addition, the system was maintained to react at this temperature for 3 hours. Then control the temperature at -10~-40℃, continue to slowly drip the solution of 2.4mL trifluoromethanesulfonic acid and 20mL tetrahydrofuran. After the addition, maintain the system...

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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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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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