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Trapezoidal polysiloxane and preparation method thereof

A polysiloxane and trapezoidal technology, applied in the field of trapezoidal polysiloxane and its preparation, can solve the problems of cumbersome synthesis process and low yield, achieve broad application prospects, high phosphorus content, and increase yield

Inactive Publication Date: 2014-08-20
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of complex synthesis process and low yield of trapezoidal polysiloxane in the prior art, provide a trapezoidal polysiloxane with excellent flame-retardant modification effect, and the operation process is simple and applicable. The preparation method with broad property and high yield

Method used

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  • Trapezoidal polysiloxane and preparation method thereof
  • Trapezoidal polysiloxane and preparation method thereof
  • Trapezoidal polysiloxane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037](1) Under nitrogen protection, 1.9g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1.9g of vinyltriethoxysilane, 0.08g of Add nitrogen diisoheptanonitrile and 10 mL dimethylformamide into the flask, and react at 120° C. for 2 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain a silane coupling agent containing a phosphaphenanthrene structure.

[0038] (2) Under the protection of nitrogen, 3g of silane coupling agent containing phosphaphenanthrene structure, 3g of 3-aminopropyltriethoxysilane, 0.1g of sodium hydroxide in methanol (0.1mg / mL), 2mL of Ionized water and 16mL of methanol were added to the flask and reacted at room temperature for 0.5 hours; then the temperature was raised to 40°C for 10 hours. After the reaction, the product was slowly dropped into methanol at a volume ratio of 1:5 to precipitate a white powder, which was filtered, washed, and dried to obtain a trapezoidal polysiloxane with a molecular ...

Embodiment 2

[0050] (1) Under the protection of argon, 2.4g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.9g vinyldimethoxysilane, 0.7g azobisiso Butyronitrile, 5mL methanol, and 5mL acetonitrile were added to the flask, and reacted at 60°C for 20 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain a silane coupling agent containing a phosphaphenanthrene structure.

[0051] (2) Under the protection of argon gas, 3g of silane coupling agent containing phosphaphenanthrene structure, 9g of 3-aminopropyltrimethoxysilane, 0.1g of potassium hydroxide in methanol solution (0.1mg / mL), 2mL Deionized water, 15 mL of acetone, 15 mL of acetonitrile and 10 mL of chloroform were added to the flask, and reacted at room temperature for 1.5 hours; then the temperature was raised to 55° C. for 7 hours. After the reaction, the product was slowly dropped into methanol at a volume ratio of 1:10 to precipitate a white powder, which was filtered, washed, and drie...

Embodiment 3

[0053] (1) Under the protection of helium, 2.06g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.9g of vinyltriethoxysilane, 0.02g of azobis Isobutyronitrile, 0.02g of azobisisoheptanonitrile and 20mL of dichloromethane were added to the flask, and reacted at 60°C for 10 hours. After the reaction, the solvent was distilled off under reduced pressure to obtain a silane coupling agent containing a phosphaphenanthrene structure.

[0054] (2) Under the protection of helium, 3 g of phosphaphenanthrene structure-containing silane coupling agent, 3 g of 3-aminopropyltrimethoxysilane, 0.1 g of potassium hydroxide in methanol (0.1 mg / mL), and 2 mL of Ionized water, 20mL ethanol and 20.5mL propanol were added to the flask and reacted at room temperature for 2 hours; then the temperature was raised to 50°C for 10 hours. After the reaction, the product was slowly dropped into a mixed solution of acetone, acetonitrile and chloroform to precipitate a white powder according to a...

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Abstract

The invention discloses trapezoidal polysiloxane and a preparation method thereof. The preparation method comprises the following steps of: preparing phosphaphenanthrene trialkoxysilane, then reasonably selecting another silane coupling agent containing an active group, adopting a direct mixed hydrolysis method and preparing the trapezoidal polysiloxane by controlling the hydrolysis rate of a system in stages. According to the preparation method, the existing process which needs to use a removal type template is abandoned, the process of removing the template in post-treatment is effectively avoided, the operation process is simplified, and the yield is improved. The proportion of phosphaphenanthrene to the active group can be controlled by controlling the adding amount of two monomers, the structure of the trapezoidal polysiloxane can be regulated and controlled against the specific application demands, and the application prospects are wider. The trapezoidal polysiloxane provided by the invention contains a large proportion of the phosphaphenanthrene structure so as to be favorable for achieving high flame resistance under low content; and the prepared trapezoidal polysiloxane contains an amino group, so that the trapezoidal polysiloxane has broad application prospects in multiple functions and high performance of polymers, synthesis and preparation of novel high polymer materials and the other aspects.

Description

technical field [0001] The invention relates to a polysiloxane, in particular to a ladder polysiloxane containing a phosphaphenanthrene structure and an amino group and a preparation method thereof. Background technique [0002] Ladder polysiloxane, as a new type of organic-inorganic hybrid polymer with a double-chain structure composed of trifunctional siloxane chains (T chains), is known for its good electrical insulation, water resistance and optical transparency. Excellent heat resistance, water resistance, weather resistance and chemical resistance, and high mechanical strength, etc., have shown broad application prospects in many cutting-edge fields such as aerospace, national defense and military. [0003] At present, the types of ladder polysiloxanes that have been reported are relatively limited, mainly including ladder polyphenylsiloxane, trapezoid polymethylsiloxane, organic bridging ladder polysiloxane, trapezoid polyepoxy silicon Oxane and ladder polyarylat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/30C08G77/26C08G73/12
Inventor 顾嫒娟叶菊华梁国正
Owner SUZHOU UNIV
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