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Preparation method of organosilicon fire retardant

A flame retardant and organosilicon technology, which is applied in the field of preparation of organosilicon flame retardants, can solve the problems of polycarbonate flame retardancy to be improved, difficult product separation, environmental pollution, etc., and achieve excellent flame retardant effect and low dosage small, significant effect

Active Publication Date: 2017-05-10
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

[0005] Most of the silicone flame retardant preparation technologies in the prior art use inorganic alkali catalysts, which are not easy to separate from the product and pollute the environment. The flame retardancy of polycarbonate still needs to be improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Preparation of composite catalyst:

[0018] Add 1,5,7-triazabicyclo[4.4.0]dec-5-ene polystyrene 50Kg in 500L reactor, N-[3,5-bis(trifluoromethyl)phenyl]-N '-[(2S)-2-pyrrolidinylmethyl]thiourea 0.015Kg, bistricyclohexyl palladium dichloride 0.02Kg, soak in 300Kg deionized water for 40h, filter and dry to obtain a composite catalyst product.

[0019] (2) Synthesis reaction: Add 100Kg of dimethylsiloxane and 3Kg of γ-aminopropylmethyldiethoxysilane into a 1000L reactor, and then add 5Kg of the composite catalyst prepared in step 1; at 50°C, After reacting for 5 hours, cool to room temperature, and then purify the product by distillation to remove unreacted monomers to obtain the product, product number M-1.

Embodiment 2

[0021] (1) Preparation of composite catalyst:

[0022] Add 1,5,7-triazabicyclo[4.4.0]dec-5-ene polystyrene 50Kg in 500L reactor, N-[3,5-bis(trifluoromethyl)phenyl]-N '-[(2S)-2-pyrrolidinylmethyl]thiourea 0.01Kg, bistricyclohexyl palladium dichloride 0.01Kg, soaked in 300Kg deionized water for 20h, filtered and dried to obtain a composite catalyst product.

[0023] (2) Synthesis reaction: Add 100Kg of dimethylsiloxane and 1Kg of γ-aminopropylmethyldimethoxysilane into a 1000L reactor, and then add 1Kg of the composite catalyst prepared in step 1; at 20°C, After reacting for 1 hour, cool to room temperature, and then purify the product by distillation to remove unreacted monomers to obtain the product. Product number M-2.

Embodiment 3

[0025] (1) Preparation of composite catalyst:

[0026] In the 500L reactor, add 1,5,7-triazabicyclo[4.4.0]dec-5-ene polystyrene 50Kg, N-[3,5-bis(trifluoromethyl)phenyl]- 0.05Kg of N'-[(2S)-2-pyrrolidinylmethyl]thiourea and 0.05Kg of bistricyclohexylpalladium dichloride were soaked in 300Kg of deionized water for 60 hours, filtered and dried to obtain a composite catalyst product.

[0027] (2) Synthesis reaction: Add 100Kg of dimethylsiloxane, 5Kg of N-(β-aminoethyl)-γ-aminopropyltriethoxysilane into a 1000L reactor, and then add 10Kg of the prepared product in step 1 The composite catalyst; after reacting at 70°C for 8 hours, cooling to room temperature, and then distilling, purifying the product to remove unreacted monomers to obtain the product, product number M-3.

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Abstract

The invention provides a preparation method of an organosilicon fire retardant. The method comprises the steps of adding dimethyl siloxane, amino silane and a composite catalyst to a reaction kettle, reacting at an optimum temperature, purifying a product through distillation and removing an unreacted monomer to obtain a product.

Description

technical field [0001] The invention relates to a preparation method of an organosilicon flame retardant. Background technique [0002] Silicone flame retardant is a new type of high-efficiency, low toxicity, anti-melt drop, environmentally friendly halogen-free flame retardant, and it is also a char-forming smoke suppressant. In addition to imparting excellent flame retardant properties to the substrate, silicone flame retardants can also improve the processing performance and heat resistance of the substrate. The research on organosilicon-based flame-retardant materials is mainly to improve the flame-retardant and smoke-suppressing effect, improve the char formation and the processing and mechanical properties of the matrix material by improving the molecular structure, increasing the relative molecular weight, and blending. The silicon-containing group has high thermal stability, oxidation stability, hydrophobicity and good flexibility. The silicon-containing group is in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/08C08G77/26C08L69/00C08L83/08
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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