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A kind of intumescent flame retardant and preparation method thereof

An intumescent flame retardant and catalyst technology, applied in the field of flame retardants and their preparation, can solve the problems of limited quantity, poor polymer compatibility, inability to effectively overcome heat resistance, etc., and achieves short synthesis cycle and raw material source. Rich and good interface binding effect

Active Publication Date: 2015-08-19
苏州沃尔兴电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, phosphorus-containing compounds are the source of acid sources, and a single linear molecular structure still cannot effectively overcome the lower heat resistance caused by phosphorus-containing groups.
Secondly, the active group contained in the flame retardant molecule is located at the end of the linear molecule, the number is limited, and the compatibility with the polymer is not good

Method used

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  • A kind of intumescent flame retardant and preparation method thereof
  • A kind of intumescent flame retardant and preparation method thereof
  • A kind of intumescent flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1. Synthesis of chlorinated spirocyclic phosphate

[0030] Under nitrogen protection, 13.6 g of pentaerythritol was added into 90 mL of phosphorus oxychloride, and the temperature was gradually raised to 80° C. for 8 h. After the reaction, wash with carbon tetrachloride and ethanol three times in sequence, filter with suction, and dry in vacuum to obtain a white powder product with a yield of 81.5%.

[0031] 2. Synthesis of amino group-containing hyperbranched polysiloxane

[0032] Under nitrogen protection and normal temperature, add 9g of deionized water, 50mL of ethanol and 0.5mL of tetraethylammonium hydroxide (20% aqueous solution) into a 250mL reactor, and stir to obtain a uniform mixed solution. 22.1 g of γ-aminopropyltriethoxysilane was added dropwise to the reactor using a constant pressure dropping funnel, and the dropwise addition was completed within 10 minutes. After raising the temperature to 50° C. for 10 hours, hexamethyldisilane was added into the rea...

Embodiment 2

[0057] 1. Synthesis of chlorinated spirocyclic phosphate

[0058] Under the protection of nitrogen, 6.8g of pentaerythritol was added into 45mL of phosphorus oxychloride, and then the temperature was gradually raised to 80°C for 8h. After the reaction, wash with carbon tetrachloride and ethanol three times successively, filter with suction, and dry in vacuum to obtain a white powder product with a yield of 79.5%.

[0059] 2. Synthesis of amino group-containing hyperbranched polysiloxane

[0060] Under nitrogen protection, at room temperature, add 18g of deionized water, 50mL of methanol and 1mL of tetraethylammonium hydroxide (20% aqueous solution) into a 250mL reactor, and stir to obtain a uniform mixture. 44.2 g of γ-aminopropyltriethoxysilane was added dropwise to the reactor using a constant pressure dropping funnel, and the dropwise addition was completed within 10 minutes. After reacting at 50°C for 12 hours, add the end-capping agent hexamethyldisilane into the reacto...

Embodiment 3

[0064] 1. Synthesis of chlorinated spirocyclic phosphate

[0065]Under the protection of nitrogen, 13.6g of pentaerythritol was added into 45mL of phosphorus oxychloride, and then the temperature was gradually raised to 80°C for 8h. After the reaction, wash with carbon tetrachloride and ethanol three times successively, filter with suction, and dry in vacuum to obtain a white powder product with a yield of 69.7%.

[0066] 2. Synthesis of amino group-containing hyperbranched polysiloxane

[0067] Under nitrogen protection, add 4.5g of deionized water, 50mL of ethanol and 0.5mL of tetramethylammonium hydroxide (20% aqueous solution) into a 250mL reactor, and stir to obtain a uniform mixture. Add 11 g of γ-aminopropyltriethoxysilane dropwise into the three-necked flask using a constant pressure dropping funnel, and the dropwise addition is completed within 10 minutes. After reacting at 50°C for 10 hours, add the end-capping agent hexamethyldisilane into the reactor, and continu...

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Abstract

The invention discloses swelling flame retardant and a preparation method thereof. Under the protection of nitrogen, hyperbranched polysiloxane containing amino groups is dissolved in acetone, and catalyst pyridine or triethylamine is added into the mixture to obtain the solution; and dichloropentate is dissolved in acetonitrile to be gradually added into the solution, and after the reaction is ended, the swelling flame retardant can be obtained through a washing step and a filtering step. The swelling flame retardant adopts the hyperbranched polysiloxane containing a great amount of nitrogen elements as a gas source, the group on the end of the hyperbranched polysiloxane of a spherical structure is combined with the dichloropentate of bifunctional end to end to form a large molecular body (netted) structure, and a great amount of active groups can be achieved; and the welling flame retardant has thermal oxygen stability and flame resistance and has application prospect on the aspects such as research and development of novel flame retardant materials, modification and high performance orientation of polymers and multiple functional groups. The preparation method is simple in process, the synthesis period is short, the yield is high, the source of raw materials is wide, and the applicability is wide.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to an intumescent flame retardant and a preparation method thereof. Background technique [0002] In recent years, intumescent flame retardants have been widely used in the research and development of flame-retardant polymer materials due to their outstanding advantages such as high flame-retardant efficiency, halogen-free, less smoke, and environmental friendliness. Intumescent flame retardants usually contain three parts: acid source, carbon source and gas source. When heated, the carbon source is dehydrated under the catalysis of the acid source to form an isolated stable carbon layer; the incombustible gas generated by the decomposition of the gas source foams, thereby forming a honeycomb-shaped expanded carbon layer between the fire source and the polymer. to the role of flame retardancy. [0003] Traditional intumescent flame retardants are mainly mixed t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/395C08G77/26C08L79/08C08L83/08
Inventor 梁国正杨成武顾嫒娟张志勇袁莉
Owner 苏州沃尔兴电子科技有限公司
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