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Phosphorus-containing flame retardant based on polyhedral oligomeric silsesquioxane (POSS) and preparation method of phosphorus-containing flame retardant

A polysilsesquioxane and flame retardant technology, which is applied in the field of flame retardant materials, can solve the problems of low flame retardant efficiency, large proportion of flame retardant silicone rubber, and low decomposition temperature.

Inactive Publication Date: 2017-05-31
SHANDONG SHIP TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These flame retardants are added in a large amount, the flame retardant efficiency is low, the decomposition temperature is low, the prepared flame retardant silicone rubber has a large proportion, the mechanical properties of the material are seriously deteriorated, and the heat resistance is poor.
In addition, flame-retardant silicone rubber also uses platinum catalysts as flame retardants. This type of flame retardant is expensive, and the effect is not obvious when used alone. Generally, phosphorus-nitrogen flame retardants should be compounded.

Method used

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  • Phosphorus-containing flame retardant based on polyhedral oligomeric silsesquioxane (POSS) and preparation method of phosphorus-containing flame retardant
  • Phosphorus-containing flame retardant based on polyhedral oligomeric silsesquioxane (POSS) and preparation method of phosphorus-containing flame retardant
  • Phosphorus-containing flame retardant based on polyhedral oligomeric silsesquioxane (POSS) and preparation method of phosphorus-containing flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Vacuum dry 216g DOPO at 110°C for 8 hours, completely dissolve the dried DOPO with N,N-dimethylformamide, put it in a high-pressure reactor, pass through nitrogen protection and mechanically stir for 3 hours;

[0029] 2) Add an isopropanol solution of chloroplatinic acid (1% mass fraction of chloroplatinic acid) into the above autoclave, raise the temperature to 80°C, and keep stirring for 0.5 hours;

[0030] 3) Slowly add 228g of VTES dropwise into the above autoclave, keep the temperature at 80°C, and keep stirring for 25 hours. To obtain a phase-separated solution, take the light yellow liquid in the upper layer, distill under reduced pressure, and remove the solvent to obtain the adduct DOPO-VTES, with a yield of 88%.

[0031] 4) Add 150g DOPO-VTES into the reaction vessel equipped with a condenser, raise the temperature to 40~80°C, add 3g of 37% concentrated hydrochloric acid dropwise, continue to stir, the stirring speed is 50r / min, the stirring time is 30h, af...

Embodiment 2

[0033] 1) Vacuum dry 216g DOPO at 110°C for 4 hours, completely dissolve the dried DOPO with isopropanol, put it in a high-pressure reactor, pass through nitrogen protection and stir mechanically for 3 hours;

[0034] 2) Add platinum-tetrahydrofuran complex into the above autoclave, raise the temperature to 90°C, and keep stirring for 0.4 hours;

[0035] 3) Slowly add 190g of VTES dropwise into the above autoclave, keep the temperature at 90°C and keep stirring for 20 hours. To obtain a phase-separated solution, take the light yellow liquid in the upper layer, distill under reduced pressure, and remove the solvent to obtain the adduct DOPO-VTES, with a yield of 80%.

[0036] 4) Add 150g DOPO-VTES into a reaction vessel equipped with a condenser, raise the temperature to 70°C, add 1.75g ​​85% concentrated phosphoric acid dropwise, continue stirring at a stirring speed of 50r / min for 20h, after cooling, suction filter to obtain a white powder, After washing with deionized water...

Embodiment 3

[0038] 1) Vacuum dry 216g DOPO at 110°C for 8 hours, completely dissolve the dried DOPO with 1,4-dioxane, put it in a high-pressure reactor, pass through nitrogen protection and stir mechanically for 3 hours;

[0039] 2) Add platinum(0)-1,3-diethylene-1,1,3,3-tetramethyldisiloxane complex into the above autoclave, raise the temperature to 85°C, and keep stirring for 0.8 hours ;

[0040] 3) Slowly add 202g of VTES dropwise into the above autoclave, keep the temperature at 85°C, and keep stirring for 25 hours. To obtain a phase-separated solution, take the light yellow liquid in the upper layer, distill under reduced pressure, and remove the solvent to obtain the adduct DOPO-VTES, with a yield of 79%.

[0041] 4) Add 150g DOPO-VTES into the reaction vessel equipped with a condenser, raise the temperature to 75°C, add 2g of 65% concentrated nitric acid dropwise, continue stirring at a stirring speed of 50r / min for 25h, after cooling, suction filter to obtain a white powder, use ...

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Abstract

The invention discloses a phosphorus-containing flame retardant based on polyhedral oligomeric silsesquioxane (POSS) and a preparation method of the phosphorus-containing flame retardant. The flame retardant is prepared by carrying out hydrogenated addition and acid-catalyzed hydrolysis condensation reaction on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and DOPO derivatives thereof and vinyltriethoxysilane (VTES); the flame retardant has the advantages of high phosphorus content, high flame-retardant efficiency, good heat resistance and little influence on mechanical property of a material; the flame retardant is used for products such as high temperature vulcanized silicone rubber and room temperature vulcanized silicone rubber, and also can be used as a temperature-resistant flame retardant of a thermoplastic polymer material; meanwhile, the flame retardant is high in phosphorus content; by adding a small amount of flame retardant, an excellent flame-retardant effect can be realized; a unique POSS structure belongs to a semi-inorganic organosilicone material, so the heat resistance of the flame retardant is improved.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant materials, and in particular relates to a cage-like polysilsesquioxane-based phosphorus-containing flame retardant for highly efficient flame-retardant silicone rubber and a preparation method thereof. Background technique [0002] Silicone rubber materials are widely used in industrial production and daily life. They have certain combustion self-extinguishing properties, but their flame retardancy is poor. High flame-retardant silicone rubber is still the focus of current research. At present, the flame retardants that can be used for silicone rubber can be divided into two categories: halogen-containing flame retardants and halogen-free flame retardants. Due to the great environmental pressure of halogen-containing flame retardants, many countries have banned their use. Burning silicone rubber is a research hotspot. [0003] The flame retardants used in halogen-free flame-retardant sili...

Claims

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Application Information

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IPC IPC(8): C08G77/30C08L83/07C08L83/08C08K9/06C08K3/36
CPCC08G77/045C08L83/04C08L2201/02C08L2201/08C08L2205/02C08L83/08C08K9/06C08K3/36
Inventor 汤飞刘增杰王新波黄玉东邱化玉李涛张孝阿
Owner SHANDONG SHIP TECH RES INST
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