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Preparation method of novel halogen-free phosphorus-nitrogen flame retardant and preparation method of flame-retardant composite material

A flame retardant composite material, halogen-free phosphorus nitrogen technology, applied in the field of preparation of flame retardant composite materials, can solve the problems of poor flame retardant performance, poor compatibility, loose carbon layer, etc., to achieve improved mechanical properties, good density, good The effect of flame retardant effect

Pending Publication Date: 2021-12-17
JIANGSU YUEKE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its poor flame retardant performance, PET is limited to be used in more demanding and special occasions. Therefore, the development of PET foam products and foam products with flame retardant function will break the foreign monopoly. In order to improve the flame retardancy of PET , so that it can be applied to more fields, and there have been many studies in recent years. At present, the most effective way to improve its flame retardancy is to add phosphorus-nitrogen flame retardants to the PET matrix, which is comparable to traditional halogen-containing flame retardants. It is more environmentally friendly than metal hydroxide flame retardants, and has higher flame retardant efficiency than metal hydroxide flame retardants; in phosphorus nitrogen flame retardants, phosphazene compounds are one of the most commonly used flame retardants, as a phosphorus nitrogen Ring non-conjugated compound, its unique phosphorus, nitrogen hybrid and higher phosphorus, nitrogen content make it have good thermal stability and flame retardancy; but the existing phosphazene compound and polymer matrix Poor compatibility, the carbon layer is loose and easy to fall off, such as PET polymers, and a large amount of phosphazene compound needs to be added to achieve a good flame retardant effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of a novel halogen-free phosphorus nitrogen flame retardant, the steps are as follows:

[0023] S1. Dissolve hexachlorocyclotriphosphazene in dimethylacetamide, add it into a 500ml four-neck round bottom flask, and heat to 70°C while stirring; use a water bath to stir and heat.

[0024] S2. Add dopamine hydrochloride and triethylamine into the round-bottomed flask, slowly stir and reflux in a water bath at 70°C for 8 hours, and the stirring rate is 200-300r / min. After the reaction is complete, the cooling product is precipitated, and the ethanol aqueous solution is used for cleaning. Centrifuge or suction filtration to filter and dry to obtain the intermediate product, wherein the molar ratio of hexachlorocyclotriphosphazene, dopamine hydrochloride and triethylamine is 1:6:1.

[0025] S3. Carry out self-polymerization of the above-mentioned intermediate product, weigh dopamine hydrochloride, and prepare a dopamine solution with a concentration of 2 ...

Embodiment 2

[0028] S1. Dissolve hexachlorocyclotriphosphazene in dimethylacetamide, add it into a 500ml four-neck round bottom flask, and heat to 70°C while stirring; use a water bath to stir and heat.

[0029] S2. Add dopamine hydrochloride and triethylamine into the round-bottomed flask, slowly stir and reflux in a water bath at 70°C for 8 hours, and the stirring rate is 200-300r / min. After the reaction is complete, the cooling product is precipitated, and the ethanol aqueous solution is used for cleaning. Centrifuge or suction filtration to filter and dry to obtain the intermediate product, wherein the molar ratio of hexachlorocyclotriphosphazene, dopamine hydrochloride and triethylamine is 1:3:1.

[0030] S3. Carry out self-polymerization of the above-mentioned intermediate product, weigh dopamine hydrochloride, and prepare a dopamine solution with a concentration of 2 g / L of dopamine hydrochloride and Tris-HCL buffer solution, and mix the intermediate product obtained in step S2 with ...

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Abstract

The invention discloses a preparation method of a novel halogen-free phosphorus-nitrogen flame retardant and a preparation method of a flame-retardant composite material. According to the invention, phosphonitrilic chloride trimer and dopamine hydrochloride are combined, a synergistic effect can be generated, the halogen-free flame-retardant effect can be achieved, the overall mechanical property of the composite material can be improved through dopamine hydrochloride, and both flame retardance and toughening are realized. Due to the fact that polydopamine with the thickness of 1-40 nm is arranged on the surface of the novel halogen-free phosphorus-nitrogen flame retardant, the compatibility of the novel halogen-free phosphorus-nitrogen flame retardant and a high polymer material is improved by taking the polydopamine as an intermediate carrier, a relatively good flame-retardant effect can be achieved by adding a small amount of the novel halogen-free phosphorus-nitrogen flame retardant, the problems of large addition amount, high cost and the like of a flame retardant are solved, the prepared flame-retardant composite material has both flame retardance and toughening, and a carbon layer generated in the combustion process is promoted to have higher strength and better density.

Description

technical field [0001] The invention relates to a preparation method of a novel halogen-free phosphorus nitrogen flame retardant and a preparation method of a flame retardant composite material. Background technique [0002] Polymer plastics can maintain excellent physical and mechanical properties in a wide temperature range. It has excellent fatigue resistance, friction resistance and aging resistance, outstanding electrical insulation, and is stable to most organic solvents and inorganic acids. Moreover, the production energy consumption is low and the processability is good, so it has been widely used in plastic packaging bottles, films and synthetic fibers, such as PET. However, due to its poor flame retardant performance, PET is limited to be used in more demanding and special occasions. Therefore, the development of PET foam products and foam products with flame retardant function will break the foreign monopoly. In order to improve the flame retardancy of PET , so t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/04C08L85/02C08G79/02C08G73/06C08L67/02
CPCC08L79/04C08G79/025C08G73/0672C08L67/02C08L2201/02C08L2201/22C08L85/02
Inventor 周利峰曹静诗李利红
Owner JIANGSU YUEKE NEW MATERIAL
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