A kind of phosphorus-silicon composite flame retardant and its preparation method and application

A technology of compounding flame retardant and phosphorous silicon, applied in the field of flame retardant materials, can solve the problems of limited application, low thermal stability, foam generation, etc., achieve low preparation and application cost, improve processing performance, prevent melting Effect

Active Publication Date: 2017-04-05
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Phosphorus-based flame retardants not only have the characteristics of high efficiency and multi-function, but also are safe and environmentally friendly. They are currently the most important substitutes for halogen-based flame retardants, but their thermal stability is low. , will generate foam in plastic and rubber, resulting in limited application

Method used

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  • A kind of phosphorus-silicon composite flame retardant and its preparation method and application
  • A kind of phosphorus-silicon composite flame retardant and its preparation method and application
  • A kind of phosphorus-silicon composite flame retardant and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Add 50g of phenyltrichlorosilane and 250ml of benzene to the round bottom flask successively, slowly add 20mL of water while stirring, and let the system stand for 10 hours after stirring at room temperature for 12 hours; use a separatory funnel to remove the acid layer at the bottom, use distilled water Or wash with an alkaline solvent to make the organic phase neutral; add 8 mL of benzyltrimethylammonium hydroxide methanol solution to the organic phase, stir and reflux for 24 hours; filter and dry to obtain the following figure 1 Caged octaphenylsilsesquioxane (POSS) of the structure shown.

[0039] Take 10g of cage-like octaphenylsilsesquioxane and place it in a round bottom flask, add 100mL of tetrahydrofuran and 4mL of 25vol% aqueous solution of tetramethylammonium hydroxide to it in turn, and reflux for 4 hours; add dilute hydrochloric acid to neutralize the reaction solution to Neutral; concentrated to remove the volatile solvent therein, to obtain a white solid;...

Embodiment 2

[0042] Add 75g of phenyltrichlorosilane and 350ml of benzene to the round bottom flask successively, slowly add 30mL of water while stirring, the system is stirred at room temperature for 16 hours and then stand for 6 hours; use a separatory funnel to remove the acid layer at the bottom, and use distilled water Or wash with an alkaline solvent to make the organic phase neutral; add 10 mL of benzyltrimethylammonium hydroxide methanol solution to the organic phase, stir and reflux for 36 hours; filter and dry to obtain the following figure 1 Caged octaphenylsilsesquioxane (POSS) of the structure shown.

[0043] Take 15g of cage-like octaphenylsilsesquioxane and place it in a round bottom flask, add 200mL of tetrahydrofuran and 6mL of 25vol% tetramethylammonium hydroxide aqueous solution to it successively, and reflux for 5 hours; add dilute hydrochloric acid to neutralize the reaction solution to Neutral; concentrated to remove the volatile solvent therein, to obtain a white sol...

Embodiment 3

[0046] Add 80g of phenyltrichlorosilane and 400ml of benzene in turn to the round bottom flask, slowly add 40mL of water while stirring, the system is stirred at room temperature for 8 hours and then stand for 12 hours; use a separatory funnel to remove the acid layer at the bottom, and use distilled water Or washing with an alkaline solvent to make the organic phase neutral; add 13mL of benzyltrimethylammonium hydroxide methanol solution to the organic phase, stir and reflux for 36 hours; filter and dry to obtain the following figure 1 Caged octaphenylsilsesquioxane (POSS) of the structure shown.

[0047] Take 20g of cage-like octaphenylsilsesquioxane and put it in a round bottom flask, add 250mL of tetrahydrofuran and 8mL of 25vol% tetramethylammonium hydroxide aqueous solution to it successively, and reflux for 6 hours; add dilute hydrochloric acid to neutralize the reaction solution to Neutral; concentrated to remove the volatile solvent therein, to obtain a white solid; t...

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Abstract

The invention discloses a phosphorus-silicon composite flame retardant as well as a preparation method and application thereof. The phosphorus-silicon composite flame retardant is a cage-like tetraphenyl trisilicate phosphorus silsesquioxane shown in the description, and the flame retardant is prepared according to the following steps: firstly hydrolyzing POSS to chipping POSS under the action of an organic alkali, and then carrying out reaction of the chipping POSS with metaphosphoric acid. Experiments show that the phosphorus-silicon composite flame retardant provided by the invention gives full play to the advantages of a silicon flame retardant and a phosphorus flame retardant, compensates defects of the silicon flame retardant and the phosphorus flame retardant, has significant synergistic flame retardance and complementarity, and excellent thermal insulation, smoke suppression and oxygen supply cutoff functions, also has the functions of protecting the environment, safety and preventing molten drop, can be directly used for preparing silicone rubber, can not only improve the flame retardance of the silicone rubber, but also perfect the thermal insulation, smoke suppression and mechanical properties of the silicone rubber, and the phosphorus-silicon composite flame retardant has the advantages of being low in preparation and application costs, easy to realize large-scale industrialized production, and the like.

Description

technical field [0001] The invention relates to a phosphorus-silicon composite flame retardant and its preparation method and application, belonging to the technical field of flame-retardant materials. Background technique [0002] At present, in the field of flame retardants for polymer materials, halogenated flame retardants are widely used. Although the flame retardant effect of this type of flame retardants is very good, due to the release of hydrogen halide gas and non-degradability when halogens burn, the current Use has been restricted. [0003] As a rising star in the flame retardant family, silicon-based flame retardants began in the early 1980s. It not only has excellent flame retardant properties such as high efficiency, low toxicity, smoke suppression, and promotion of char formation, but also has significantly improved processing performance and mechanical properties compared with traditional flame retardants, and is well received by the public. favored by man...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L83/04C08K5/549C07F9/6561
Inventor 袁章林王锦成韦小凤李涛涛庹文海
Owner SHANGHAI UNIV OF ENG SCI
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