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Hyperbranched POSS flame retardant and preparation method and applications thereof

A flame retardant, flame retardant composite material technology, applied in the field of flame retardant materials, can solve the problems of poor polymer compatibility, poor flame retardant effect, limited improvement of polymer flame retardant effect, etc., to achieve good compatibility, Strong practical value, excellent heat insulation and smoke suppression effect

Active Publication Date: 2016-12-14
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the above use, although the addition of POSS can improve the flame retardancy of polymer materials to a certain extent, there are still defects such as poor flame retardancy and poor compatibility with polymers, so the improvement of polymer flame retardancy is limited.
At present, there is no relevant report on the use of hyperbranched polymers to modify POSS to prepare hyperbranched POSS flame retardants, and there is no relevant report on applying the prepared hyperbranched POSS flame retardants to rubber materials to prepare flame-retardant rubber.

Method used

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  • Hyperbranched POSS flame retardant and preparation method and applications thereof
  • Hyperbranched POSS flame retardant and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. AB 2 Monomer preparation:

[0032] Under the protection of nitrogen, take 0.10mol 1,3,5-trichlorobenzene and place it in a four-neck flask, add 0.10mol tetrahydrofuran and 2.4g metal magnesium to it in turn, mix and stir at room temperature for 20 minutes, then raise the temperature to 30 ℃, heat preservation and stirring for 1 hour, a colorless transparent liquid is obtained, which is AB 2 Monomer: 1,3-dichlorobenzene-5-magnesium monochloride.

[0033] Two, the preparation of heptaphenyl trisilanol silsesquioxane:

[0034] Take 20g of clathrate-shaped octaphenylsilsesquioxane (POSS for short) and place it in a four-neck flask, add 100mL of tetrahydrofuran and 8mL of an aqueous solution with a mass fraction of 25% tetramethylammonium hydroxide to it in turn, and stir the reaction at 60°C 3 hours; finish the reaction, cool the reaction solution to room temperature, then dropwise add dilute hydrochloric acid to neutralize the reaction solution to neutrality; concent...

Embodiment 2

[0047] 1. AB 2 Monomer preparation:

[0048] Under the protection of nitrogen, take 0.20mol 1,3,5-trichlorobenzene and place it in a four-neck flask, add 0.20mol tetrahydrofuran and 4.8g metal magnesium to it in turn, mix and stir at room temperature for 30 minutes, and then raise the temperature to 40 ℃, heat preservation and stirring for 1 hour, a colorless transparent liquid is obtained, which is AB 2 Monomer: 1,3-dichlorobenzene-5-magnesium monochloride.

[0049] Two, the preparation of heptaphenyl trisilanol silsesquioxane:

[0050] Take 30g of clathrate-shaped octaphenylsilsesquioxane (POSS for short) and place it in a four-neck flask, add 200mL of tetrahydrofuran and 10mL of an aqueous solution with a mass fraction of 30% tetramethylammonium hydroxide to it, and stir at 65°C 2.5 hours; finish the reaction, cool the reaction solution to room temperature, then dropwise add dilute hydrochloric acid to neutralize the reaction solution to neutrality; concentrate and remov...

Embodiment 3

[0063] 1. AB 2 Monomer preparation:

[0064] Under the protection of nitrogen, take 0.30mol 1,3,5-trichlorobenzene and place it in a four-neck flask, add 0.30mol tetrahydrofuran and 7.2g metal magnesium to it in turn, mix and stir at room temperature for 40 minutes, and then raise the temperature to 50 ℃, heat preservation and stirring for 1 hour, a colorless transparent liquid is obtained, which is AB 2 Monomer: 1,3-dichlorobenzene-5-magnesium monochloride.

[0065] Two, the preparation of heptaphenyl trisilanol silsesquioxane:

[0066] Take 40g of clathrate octaphenylsilsesquioxane (POSS for short) and place it in a four-necked bottle, add 300mL of tetrahydrofuran and 12mL of an aqueous solution with a mass fraction of 35% tetramethylammonium hydroxide to it, and stir the reaction at 70°C 3 hours; finish the reaction, cool the reaction solution to room temperature, then dropwise add dilute hydrochloric acid to neutralize the reaction solution to neutrality; concentrate an...

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Abstract

The invention discloses a hyperbranched POSS flame retardant and a preparation method and applications thereof. The hyperbranched POSS flame retardant is prepared by the following steps: performing hydrolysis reaction on octaphenyl polyhedral silsesquioxane under alkaline condition to obtain heptaphenyl trisilihydroxyl polyhedral silsesquioxane, then reacting the heptaphenyl trisilihydroxyl polyhedral silsesquioxane with 1,3,5-trichlorobenzene to obtain a hyperbranched POSS intermediate, finally reacting the obtained hyperbranched POSS intermediate with AB2 monomer. Through tests, the flame retardance performance, mechanical performance, heat-insulating and smoke inhibition performances of a silicon rubber flame-retardant composite material of the hyperbranched POSS flame retardant are obviously improved, so that the hyperbranched POSS flame retardant has wide application prospects. In addition, the preparation technique is economic and practical, the preparation process is simple, the cost is low, special equipment and harsh conditions are not needed, large-scale production is easily realized, and high practical values can be achieved.

Description

technical field [0001] The invention relates to a flame retardant and its preparation method and application, in particular to a hyperbranched POSS flame retardant and its preparation method and application, and belongs to the technical field of flame retardant materials. Background technique [0002] In the field of flame retardants for polymer materials, halogenated flame retardants are mostly used. Although this type of flame retardant has a better flame retardant effect, due to the release of hydrogen halide gas when the halogen burns, it will cause harm to people escaping from the fire scene. Serious injury, has been restricted in many European and American countries. [0003] Caged oligomeric silsesquioxane (POSS) is a new type of nanoparticle with a three-dimensional structure, and its molecular structure has a skeleton diameter of 1-3nm. It is a new type of organic-inorganic hybrid material. It has the advantages of good thermal stability, high strength, and high ri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08L83/04C08L83/05C08L83/07
CPCC08G77/045C08L83/04C08L2201/02C08L2201/08C08L2205/025C08L2205/03
Inventor 李智杰王锦成
Owner SHANGHAI UNIV OF ENG SCI
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