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Biphenol polyphosphate fire retardant and preparation method and application thereof

The technology of biphenyl diphenol polyphosphate and tolyl dichlorophosphate is applied in the field of polymer type phosphorus-containing flame retardant and its preparation, and can solve the problem of flame retardant exuding flame retardant performance, decline, use and storage. and inconvenient transportation to achieve the effect of good flame retardant effect, wide application range and excellent durability

Active Publication Date: 2012-11-21
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphorus-based flame retardants currently used in large quantities such as resorcinol (diphenyl phosphate) Resorcin bis (diphenyl phosphate) flame retardant, referred to as RDP, and bisphenol-A (diphenyl phosphate) Bisphenol-A Bis (Diphenyl Phosphate) ), referred to as BDP is a viscous oily liquid, which is extremely inconvenient in the process of use, storage and transportation.

Method used

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  • Biphenol polyphosphate fire retardant and preparation method and application thereof
  • Biphenol polyphosphate fire retardant and preparation method and application thereof
  • Biphenol polyphosphate fire retardant and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0022] Put 186g of biphenol and 1.33g of aluminum chloride into a four-necked flask equipped with a condenser, a stirrer, a thermometer and a protective gas inlet and outlet, pass in nitrogen, stir and raise the temperature to 60°C, and drop gradually within half an hour Add 225 grams of p-cresyl dichlorophosphate, keep the temperature for reaction for 4 hours, then raise the temperature to 200°C and react for 3 hours until no HCl gas escapes (reaction ends). After cooling, 300ml of chloroform was added to dissolve it completely, and then poured into 8 times the volume of anhydrous methanol for precipitation. After filtration and vacuum drying, 320g of white powdery solid was obtained, with a yield of 94%. The weight average molecular weight of the obtained flame retardant was 29045 through gel chromatography detection.

Embodiment 2

[0024] Put 167.4g of biphenyldiphenol and 2.72g of zinc chloride into a four-necked flask equipped with a condenser, a stirrer, a thermometer and a protective gas inlet and outlet, feed in nitrogen, stir and raise the temperature to 70°C, gradually within half an hour Add 314 g of p-cresyl dibromophosphate dropwise, keep the temperature for reaction for 4 hours, then raise the temperature to 200° C. and react for 4 hours until no HBr gas escapes (reaction ends). After cooling, 300ml of tetrahydrofuran was added to dissolve it completely, and then poured into 10 times the volume of deionized water for precipitation. After filtration and vacuum drying, 278g of white powdery solid was obtained, with a yield of 91%. The weight-average molecular weight of the obtained flame retardant was 26322 as detected by gel chromatography.

Embodiment 3

[0026] Put 205g of biphenyldiphenol and 2.19g of calcium chloride into a four-necked flask equipped with a condenser, agitator, a thermometer and a protective gas inlet and outlet, pass in nitrogen, stir and raise the temperature to 60°C, and drop gradually within half an hour Add 225 grams of p-cresyl dichlorophosphate, keep the temperature for reaction for 1 hour, then raise the temperature to 200°C for reaction for 4 hours, until no HCl gas escapes (reaction ends). After cooling, 300ml of dimethyl sulfoxide was added to dissolve it completely, and then poured into 8 times the volume of anhydrous methanol for precipitation. After filtration and vacuum drying, 307g of white powdery solid was obtained, with a yield of 90%. The weight-average molecular weight of the obtained flame retardant was 26015 through gel chromatography detection.

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Abstract

The invention discloses a biphenol polyphosphate fire retardant which is characterized in that n is an integer ranged from 300 to 1000. The preparation method comprises the following steps: weighing p-methyl phenyl dichlorophosphate or p-methylphenyl dibromo phosphate and biphenol based on mol ratio of 1:(0.9-1.2), and catalyst and biphenol based on mol ratio of 0.001 to 0.01; adding the weighed biphenol and catalyst to a reacting device; agitating and heating to 60-70 DEG C; adding p-methyl phenyl dichlorophosphate or p-methylphenyl dibromo phosphate within half an hour; keeping the temperature for 1 to 4 hours; and then heating to 200 DEG C to react for 3 to 4 hours to obtain white solid fire retardant; adding solvent to the prepared white fire retardant to completely dissolve; and then precipitating through the precipitating agent which is 5 to 10 times the amount of the solvent; and filtering; and finally drying in vacuum to obtain the white solid product. The biphenol polyphosphate fire retardant disclosed by the invention can be well compatible with a polymer base, is hard to shift, and has an excellent durable performance.

Description

technical field [0001] The invention belongs to the technical field of polymer-type phosphorus-containing flame retardants, and in particular relates to a class of polymer-type phosphorus-containing flame retardants and a preparation method thereof. Background technique [0002] Phosphorus-based flame retardants have the advantages of low smoke and non-toxicity, and are one of the most important types of flame retardants among all kinds of flame retardants. Its structure does not contain halogen, which can avoid the environmental problems of halogen flame retardants, and has a good development prospect. Phosphorus-based flame retardants currently used in large quantities such as resorcinol (diphenyl phosphate) Resorcin bis (diphenyl phosphate) flame retardant, referred to as RDP, and bisphenol-A (diphenyl phosphate) Bisphenol-A Bis (Diphenyl Phosphate) ), referred to as BDP is a viscous oily liquid, which is extremely inconvenient in the process of use, storage and transpor...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L67/00C08L69/00C08L77/02C08L63/00C08L85/02
Inventor 班大明秦好丽赵欧张永航刘真美韦万丽
Owner GUIZHOU NORMAL UNIVERSITY
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