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Halogen-free non-phosphorus silicon-containing flame retardant and preparation method thereof

A silicon flame retardant and catalyst technology, applied in the field of flame retardant and its preparation, can solve the problem of narrow processing window of modified bismaleimide resin, poor storage stability of hyperbranched polysiloxane, amino and imide The problem of fast reactivity of amine ring, etc., to achieve the effect of being conducive to large-scale application, good storage stability, and environmental friendliness

Active Publication Date: 2015-02-25
山东众甫新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, the storage stability of the hyperbranched polysiloxane of this amino functional group is poor, is easy to gel; The reactivity of amino group and imide ring is faster simultaneously, makes the processing window of modified bismaleimide resin narrow, not easy Facilitate large-scale production

Method used

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  • Halogen-free non-phosphorus silicon-containing flame retardant and preparation method thereof
  • Halogen-free non-phosphorus silicon-containing flame retardant and preparation method thereof
  • Halogen-free non-phosphorus silicon-containing flame retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] in N 2 Under protection, 5.19g of maleic anhydride was dissolved in 100mL of toluene to form solution A; 11.7g of γ-aminopropyltriethoxysilane was added dropwise to the toluene solution within 30 minutes, and reacted at room temperature for 0.5 hours to form Solution B.

[0037] Add 7.2g of anhydrous zinc chloride to solution B, and after the temperature reaches 80°C, add 8.52g of hexamethyldisilazane dropwise within 30 minutes. After the dropwise addition, react at 80°C for 4h, filter, and distill under reduced pressure to obtain solution C.

[0038] Add solution C, 1.14g deionized water and 0.01g tetramethylammonium hydroxide to ethanol, and reflux at 55°C for 3h. After the reaction was completed, the halogen-free, phosphorus-free and silicon-containing flame retardant was obtained by distillation under reduced pressure and vacuum drying. The number average molecular weight was 3080, the degree of branching was 0.52, and the yield was 70%. Its infrared spectrogram,...

Embodiment 2

[0054] in N 2 Under protection, 5.88g of maleic anhydride was dissolved in 100mL of toluene to form solution A; 13.3g of γ-aminopropyltriethoxysilane was added dropwise to the toluene solution within 20min, and then reacted at room temperature for 1h to form a solution b.

[0055] Add 8.2g of anhydrous zinc chloride to solution B, and after the temperature reaches 70°C, add 9.2g of hexamethyldisilazane dropwise within 30min. After the dropwise addition, react at 80°C for 4h, filter, and distill under reduced pressure to obtain solution C.

[0056] Add solution C and 1.4g deionized water into ethanol (adjust pH=10 with NaOH), and reflux at constant temperature at 55°C for 4h. After the reaction was completed, the halogen-free, phosphorus-free and silicon-containing flame retardant was obtained by distillation under reduced pressure and vacuum drying. The number average molecular weight was 3225, the degree of branching was 0.55, and the yield was 68%.

Embodiment 3

[0058] in N 2 Under protection, 15.8g of maleic anhydride was dissolved in 250mL of toluene to form solution A; a mixture of 15.1g of γ-aminopropyltriethoxysilane and 20g of γ-aminopropyltrimethoxysilane was added dropwise within 30min Toluene solution, and then react at room temperature for 0.5h to form solution B.

[0059] Add 21.6g of anhydrous zinc chloride to solution B, and after the temperature reaches 70°C, add 25.56g of hexamethyldisilazane dropwise within 25 minutes. After the dropwise addition, react at 70°C for 5h, filter, and distill under reduced pressure to obtain solution C.

[0060] Add solution C, 3.4g deionized water and 0.05g tetramethylammonium hydroxide into methanol, and reflux at 55°C for 4h. After the reaction was completed, the halogen-free, phosphorus-free and silicon-containing flame retardant was obtained by distillation under reduced pressure and vacuum drying. The number average molecular weight was 2988, the degree of branching was 0.52, and t...

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Abstract

The invention discloses a halogen-free non-phosphorus silicon-containing flame retardant and a preparation method thereof. The flame retardant is a hyperbranched silicon resin containing multiple maleimide groups, has the branching degree of 0.5-0.6 and the molecular weight of 2500-3400 and is liquid at normal temperature. The preparation method comprises the following steps: synthesizing a trialkyl silane solution containing maleimide, performing controlled hydrolysis, and performing suction filtration, reduced pressure distillation and drying, thereby obtaining the halogen-free non-phosphorus silicon-containing flame retardant. The flame retardant contains the maleimide groups and can be copolymerized with an imide ring at a certain temperature, good interaction is obtained when the reactivity is controlled, and the storage stability, reactivity control and flame retardant property of the modified resin are fully exerted. The flame retardant contains multiple maleimide groups and a flexible Si-O-Si chain, so that the modified resin has the outstanding advantages of rigidity, toughness and heat resistance. The preparation method of the flame retardant is environment-friendly, simple, feasible, short in synthesis period, rich in raw material source, wide in applicability and high in yield.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a halogen-free, phosphorus-free and silicon-containing flame retardant and a preparation method thereof. Background technique [0002] With the development of the synthetic material industry and the continuous expansion of application fields, flame retardants have broad market prospects in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, and basic necessities of life. With the increasing market competition and human awareness of environmental protection, flame retardants are developing toward the trend of halogen-free. [0003] Phosphorus-based flame retardants have the characteristics of low toxicity, low dosage and high efficiency, so they have received widespread attention as halogen-free flame retardants. However, with the deepening of research and development, it h...

Claims

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Application Information

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IPC IPC(8): C08G77/26C08G77/06C08L83/08C08L79/08
Inventor 顾嫒娟蒋志俊梁国正袁莉
Owner 山东众甫新材料有限公司
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