A kind of preparation method of phosphorus organosilicon type flame retardant

A technology of organosilicon and flame retardants, which is applied in the field of preparation of phosphorus-based organosilicon flame retardants, can solve the problems of affecting the physical properties of materials, poor use effects, and poor flame retardant properties, and achieves obvious flame retardant effects, Low cost and improved physical properties

Active Publication Date: 2021-05-28
普信氟硅新材料(衢州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The silicone flame retardant prepared by the above invention and the prior art has the disadvantage of poor compatibility with plastic materials such as PP, PS, PE, etc. It not only has poor flame retardancy, but also affects the physical properties of these materials, and the use effect is not good.

Method used

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  • A kind of preparation method of phosphorus organosilicon type flame retardant
  • A kind of preparation method of phosphorus organosilicon type flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of a phosphorus-based organosilicon type flame retardant is carried out according to the following scheme:

[0021] In terms of parts by mass, 20 parts of p-aminophenyldimethoxysilane, 35 parts of diethoxysilane and 100 parts of toluene, 0.03 parts of tris[N,N-bis(trimethylsilane)amine] Add erbium into the pressure reactor, control the temperature at 50°C, stir for 35 minutes, then pump inert gas through the reactor for 3 times after vacuuming, and add 1.5 parts of water and 2.5 parts of porous boron-containing organic base solid catalyst to the reaction kettle after removing the air. In the kettle, stir and heat up to 70°C, keep warm for 24 hours; after the reaction is completed, heat up to 113°C, use a water separator to separate the water, and then slowly add 40 parts of toluene solution containing 5.8 parts of phosphorus oxychloride to the reaction kettle , then add 0.01 part of tetramethylguanidine perfluoroethane sulfonate, control the tempera...

Embodiment 2

[0027] A preparation method of a phosphorus-based organosilicon type flame retardant is carried out according to the following scheme:

[0028] In terms of parts by mass, 10 parts of p-aminophenyldimethoxysilane, 30 parts of diethoxysilane and 80 parts of toluene, 0.01 part of tris[N,N-bis(trimethylsilane)amine] Add erbium into the pressure reactor, control the temperature at 40°C, stir for 30 minutes, then pump inert gas through the reactor for 3 times after vacuuming, and add 0.5 parts of water and 0.1 part of porous boron-containing organic base solid catalyst to the reaction kettle after removing the air. In the kettle, stir and raise the temperature to 60°C, keep the temperature for 18h; after completing the reaction, raise the temperature to 110°C, use a water separator to separate the water, and then slowly add 20 parts of toluene solution containing 3.5 parts of phosphorus oxychloride to the reaction kettle , then add 0.06 part of tetramethylguanidine perfluoroethane s...

Embodiment 3

[0034]A preparation method of a phosphorus-based organosilicon type flame retardant is carried out according to the following scheme:

[0035] According to the number of parts by mass, 30 parts of p-aminophenyldimethoxysilane, 40 parts of diethoxysilane and 120 parts of toluene, 0.06 parts of tris[N,N-bis(trimethylsilane)amine] Add erbium into the pressure reactor, control the temperature at 60°C, stir for 40 minutes, then pump inert gas through the reactor for 3 times after vacuuming, and add 3.5 parts of water and 5 parts of porous boron-containing organic base solid catalyst to the reaction kettle after removing the air. In the kettle, stir and heat up to 80°C, keep the temperature for 30h; after completing the reaction, heat up to 115°C, use a water separator to separate the water, and then slowly add 50 parts of toluene solution containing 10.6 parts of phosphorus oxychloride to the reaction kettle , then add 0.06 part of tetramethylguanidine perfluoroethane sulfonate, co...

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Abstract

The invention relates to the field of fine chemical industry, in particular to a method for preparing a phosphorus-based organosilicon flame retardant; in the method, a certain proportion of p-aminophenyltrimethoxysilane and diethoxysiloxane The alkane is fully reacted in the solvent; then the water in the reaction solution and unreacted monomers are distilled off to obtain a mixed solution, and then a quantitative amount of phosphorus oxychloride is added dropwise to the mixed solution, and the solvent is extracted after the reaction to obtain a phosphorus-based organic compound. Silicon-type flame retardant, the phosphorus-based organosilicon-type flame retardant of the present invention has good compatibility with plastic materials such as PP, PS, and PE, and has wide adaptability. It can not only endow plastic materials with good flame-retardant properties, but also can Improve the physical properties of plastic materials. Moreover, the preparation process of the invention is simple and easy to obtain, the flame retardant effect is obvious, and the addition amount is small, so it also has the advantage of lower cost.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation method of a phosphorus-based organosilicon flame retardant. Background technique [0002] Silicone flame retardant is a new type of high-efficiency, low-toxic, environmentally friendly halogen-free flame retardant, and it is also a carbon-forming smoke suppressant. It can not only endow the material with excellent flame retardant properties, but also improve the processing performance and heat resistance of the substrate. Therefore, as a new type of flame retardant, it has been developed rapidly in recent years. [0003] CN102558750A discloses a silicone flame retardant for ABS and a preparation method thereof, relating to a flame retardant. Provide a kind of silicone flame retardant for ABS, which has good compatibility with ABS, and has the characteristics of little influence on the mechanical properties of ABS, less additive amount, and excellent flame retardant pe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/395C08G77/26C08L83/08C08L23/12
Inventor 王荣军吴健泳
Owner 普信氟硅新材料(衢州)有限公司
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