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Hyperbranched polysiloxane containing phosphaphenanthrene structure and preparation method thereof

A technology of polysiloxane and phosphaphenanthrene, which is applied in the field of hyperbranched polysiloxane and its preparation, can solve the problems of no modification and affecting the heat resistance of polymers, and achieve improved compatibility and huge applications Potential, the effect of simple operation process

Inactive Publication Date: 2013-08-07
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, phosphorus-containing flame retardants generally have no modification effect on the mechanical properties of polymers, and will also affect the heat resistance of polymers.

Method used

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  • Hyperbranched polysiloxane containing phosphaphenanthrene structure and preparation method thereof
  • Hyperbranched polysiloxane containing phosphaphenanthrene structure and preparation method thereof
  • Hyperbranched polysiloxane containing phosphaphenanthrene structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under the conditions of anhydrous and nitrogen protection, 23.6g 3-glycidyl etheroxypropyltrimethoxysilane and 21.6g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide After mixing evenly, add 0.45g of catalyst triphenylphosphine, add 100g of n-propanol, heat up to 95°C and keep condensing and refluxing to continue the reaction for 6 hours; after the reaction is completed, remove the solvent by distillation under reduced pressure, remove the catalyst by filtration, and carry out vacuum drying. A transparent trialkoxysilane containing a phosphaphenanthrene structure and a hydroxyl group is obtained.

[0028] Take all the above-mentioned trialkoxysilanes containing phosphaphenanthrene structures and hydroxyl groups, 2.0g phenyltrimethoxysilane and 2.2g distilled water and mix evenly, then add 2.5mL of 4mol / L hydrochloric acid, heat to 50°C and continue the reaction for 4 hours. Distillation under reduced pressure obtains crude product;

[0029] After the crude product is...

Embodiment 2

[0037] Under the conditions of anhydrous and nitrogen protection, 24.8g 3-glycidyl etheroxypropylmethyldiethoxysilane and 21.6g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10 -After the oxides are mixed evenly, add 1.4g of catalyst triphenylphosphine, add 100g of methanol, raise the temperature to 100°C and keep condensing and refluxing to continue the reaction for 10 hours; after the reaction is completed, carry out vacuum drying, distill under reduced pressure to remove the solvent, and filter to remove the catalyst , to obtain a transparent trialkoxysilane containing a phosphaphenanthrene structure and a hydroxyl group.

[0038] Take all the above-mentioned trialkoxysilanes containing phosphaphenanthrene structure phenyl and hydroxyl groups, 20g of phenyltrimethoxysilane and 5.8g of distilled water and mix evenly, add 7.5mL of 4mol / L hydrochloric acid, heat to 60°C and continue to react for 7 hours , distillation under reduced pressure obtains crude product;

[0039] After t...

Embodiment 3

[0041] Under the conditions of anhydrous and nitrogen protection, 24.6g 2-(3,4-epoxycyclohexanealkyl)ethyltrimethoxysilane and 21.6g 9,10-dihydro-9-oxa-10- After the phosphaphenanthrene-10-oxide is mixed evenly, add 1.3g of catalyst triphenylphosphine, add 100g of ethanol, raise the temperature to 97°C and keep condensing and refluxing to continue the reaction for 8 hours; after the reaction is completed, carry out vacuum drying, and distill under reduced pressure to remove the solvent , and remove the catalyst by filtration to obtain a transparent trialkoxysilane containing a phosphaphenanthrene structure and a hydroxyl group.

[0042] Take all the above-mentioned trialkoxysilanes containing phenyl and hydroxyl groups of the phosphaphenanthrene structure, 24g of phenyltriethoxysilane and 3.5g of distilled water, mix evenly, add 7.5mL of 4mol / L hydrochloric acid, heat to 60°C and continue the reaction for 7 Hour, underpressure distillation obtains crude product;

[0043] Afte...

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Abstract

The invention discloses hyperbranched polysiloxane containing a phosphaphenanthrene structure and a preparation method thereof. The preparation method comprises the following steps of: under the water-free condition, mixing trialkoxysiloxane containing epoxide groups with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, adding triphenylphosphine serving as catalyst, dissolving the triphenylphosphine serving as catalyst in an alcohol solvent, and obtaining the trialkoxysiloxane containing the phosphaphenanthrene structure and hydroxyl radicals; mixing the trialkoxysiloxane with trialkoxysiloxane containing phenyl groups, dissolving the mixture into distilled water, adding catalysts such as hydrochloric acid and the like dropwise, carrying out purification, filtering, reduced-pressure distillation and vacuum drying on raw products and obtaining the hyperbranched polysiloxane containing the phosphaphenanthrene structure, the phenyl groups and the hydroxide radicals. The hyperbranchedpolysiloxane integrates the molecular characteristics of the hyperbranched polysiloxane, the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, the phenyl groups and the hydroxide radicals, and canbe applied to modification of polymers. The preparation method provided by the invention has the characteristics of wide applicability and simple operation process.

Description

technical field [0001] The invention relates to a hyperbranched polymer and a synthesis method thereof, in particular to a hyperbranched polysiloxane containing a phosphaphenanthrene structure and a preparation method thereof. Background technique [0002] Flame retardants have become one of the important components in the preparation of flame retardant polymer materials. Flame retardants are mainly divided into inorganic flame retardants and organic flame retardants. The application of inorganic flame retardants is greatly limited due to the disadvantages of large amount of addition, low flame retardant efficiency, single flame retardant mechanism, and poor compatibility with polymers. There are many kinds of organic flame retardants, which can be selected and designed according to different conditions of use, so they have attracted people's attention. [0003] Silicone flame retardant is a "rising star" in the flame retardant family. It not only has the advantages of hig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/30
Inventor 梁国正张志勇顾嫒娟缪承赟陈桐陈倩袁莉
Owner SUZHOU UNIV
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