Non-halogen polymer-type additive resisting smelting-dropping and combustion, and its preparing process and usage

A technology of additives and polymers, applied in the direction of fire-resistant coatings, etc., can solve the problems of poor droplet resistance and cannot meet the requirements of droplet resistance and flame retardancy at the same time, and achieve good char formation, good application prospects, good compatibility

Inactive Publication Date: 2002-10-30
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But no matter adopting that kind of mode to carry out flame retardant, the research focus of prior art all is to put on the flame retardant aspect of polymer, but pays little attention to the droplet resistance of polymer, which makes most oxygen index Flame-retardant polymers with high evaluation by determination methods have poor droplet resistance, such as the "flame-retardant polyester composition" disclosed in Japanese Patent No. 47-32299, German Patent DE-OS 2438967, DE-OS 2253207 and DE-OS 213235 respectively disclose flame-retardant polyester shaping compositions containing large molecular weight organic phosphine compounds, flame-retardant thermoplastic polyester resins containing aryl phosphides, and phosphorus-containing flame-retardant poly(propylene terephthalate) additives etc., cannot meet the requirements for droplet resistance and flame retardancy at the same time

Method used

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  • Non-halogen polymer-type additive resisting smelting-dropping and combustion, and its preparing process and usage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This embodiment is the preparation of polythiophenylphosphonic acid bis-p-hydroxyphenyl sulfone ester, and its reaction formula is:

[0023] Add 1 mol of thiophenylphosphonic acid dichloride, 1 mol of bisphenol S and 0.08 mol of calcium chloride into a 500 ml multi-neck flask equipped with a stirring device and nitrogen inlet and outlet, then feed nitrogen and gradually heat up while stirring Heat it to 250°C, let it melt and react for 3 hours; after the reaction is finished and cooled, add chloroform until the reactant is completely dissolved, then pour it into methanol whose volume is 5 times or more than that of the reactant solution to precipitate, and precipitate a white powdery product. The white powdery product is suction-filtered from the co-precipitant methanol, and then dried. The drying can be natural air drying or drying, preferably vacuum drying. The yield of this example is 99%, and the melting temperature of the product is 180°C.

Embodiment 2

[0025] This embodiment is the preparation of 2.2-bis-p-hydroxyphenylpropane polythiophenylphosphonate, and its reaction formula is:

[0026] Put 1 mol of thiophenylphosphonic acid dichloride, 1 mol of bisphenol A and 0.05 mol of calcium chloride in a 500 ml multi-neck bottle equipped with a stirring device and nitrogen inlet and outlet, then feed nitrogen and gradually heat under stirring Raise the temperature to 200°C, let it melt and react for 5 hours, then increase the temperature to 250°C and react for 3 hours; after the reaction is finished and cooled, add benzyl alcohol until the reactant is completely dissolved, and then pour in a volume that is 5 times or more than the volume of the reactant solution Precipitate in absolute ethanol to precipitate a white powdery product; filter the white powdery product from the co-precipitant absolute ethanol, and then dry it. The yield is 90%, and the melting temperature of the product is 140°C.

Embodiment 3

[0028] This embodiment is the preparation of polythiophenylphosphonic acid bis-p-hydroxyphenyl sulfone ester, and its reaction formula is:

[0029] In a 500ml multi-neck bottle equipped with a stirring device and a nitrogen inlet and outlet, first add 0.5mol bisphenol S and 0.03mol aluminum chloride, then feed nitrogen and gradually heat up to 230°C under stirring to melt it , then add 0.55mol thiophenylphosphonic acid dichloride dropwise, and control the dropping time for 1 hour. After the dropwise addition is completed, react for 3 hours; Precipitate in methanol with a volume of 5 times or more of the product solution, and precipitate a white powdery product; filter the white powdery product from the co-precipitant methanol, and then dry it. The yield is 95%, and the melting temperature of the product is 180°C.

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Abstract

A non-halogen polymer type additive for resisting fusion dropping and firing is prepared from arylthiophosphonic dihalogen and diphenol compounds in mole ratio of 1:(0.9-1.1) through fusing and polycondensating, and can be used to synthesize polyester or polyamide compounds by polycondensation. Its advantages include high chairing performance, fusion dropping resistance and flame-retarding efficiency, good compatibility to polymer substrate, and environmental pollution.

Description

1. Technical field [0001] The invention belongs to the technical field of anti-droplet additives and flame retardants and their preparation methods and applications. Specifically, the invention is a kind of anti-droplet effect that is particularly remarkable, and also has a flame-retardant effect, which can replace the existing polymer additives. Additive flame retardants such as esters, especially halogen-free polymer additives containing halogen additive flame retardants, as well as the preparation method of this additive and its use in polyester and polyamide polymers for anti-melting drops and Flame retardant use. 2. Background technology [0002] Most of the existing polymers, such as polyester, polyamide, etc., generally do not have flame retardancy, but with the expansion of their application fields, in some special occasions, such as decoration of aviation, entertainment places, homes, etc. In terms of materials or protective clothing used in special industries, it ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/14
Inventor 王玉忠班大明吴博
Owner SICHUAN UNIV
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