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ODOPB (10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide)-base polyphosphate flame retardant, and preparation method and application thereof

A technology based on polyphosphate and phenyl dichlorophosphate, applied in the field of polymer type phosphorus-containing flame retardant and its preparation, can solve the problem of liquid flame retardant exuding flame retardant performance, decline, use, storage and transportation Inconvenience and other problems, to achieve the effect of good flame retardant effect, wide application range and excellent durability

Inactive Publication Date: 2012-11-28
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 are viscous oily liquids, which are extremely inconvenient in the process of use, storage and transportation. At the same time, liquid flame retardants are easy to seep out of the matrix, resulting in a decrease in flame retardant performance.

Method used

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  • ODOPB (10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide)-base polyphosphate flame retardant, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 292g of ODOPB 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 140°C, and gradually add phenyl 210 grams of dichlorophosphate, keep the temperature for reaction for 1 hour, then raise the temperature to 200°C for reaction for 2 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 n-hexane for precipitation. After filtration and vacuum drying, 390g of white powdery solid was obtained, with a yield of 95%. The weight average molecular weight of the obtained flame retardant was 152085 through gel chromatography detection.

Embodiment 2

[0024] Put 324g of ODOPB 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, pass in nitrogen, stir and raise the temperature to 140°C, and gradually add phenyl 314 grams of dibromophosphate, keep the temperature for reaction for 2 hours, then raise the temperature to 210° C. and react for 3 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, 450g of white powdery solid was obtained, with a yield of 97%. The weight average molecular weight of the obtained flame retardant was 156552 through gel chromatography detection.

Embodiment 3

[0026] Put 389g of ODOPB and 2.19g of calcium 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 140°C, and gradually add p-toluene dropwise within half an hour 225 grams of dichlorophosphate, keep the temperature for reaction for 1 hour, then raise the temperature to 220°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, 429g of white powdery solid was obtained, with a yield of 90%. The weight average molecular weight of the obtained flame retardant was 136088 through gel chromatography detection.

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Abstract

The invention discloses an ODOPB (10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide)-base polyphosphate flame retardant which is characterized in that n is a whole number ranging from 2000 to 4000, and Y is a hydrogen atom or alkyl group of which the carbon atom number is less than 6. The preparation method comprises the following steps: weighing phenyldichlorophosphate or phenyl dibromophosphate, ODOPB and a catalyst, wherein the mol ratio of phenyldichlorophosphate or phenyl dibromophosphate to ODOPB is 1:(0.9-1.2), and the mol ratio of catalyst to ODOPB is 0.001-0.01; adding the ODOPB and the catalyst into a reactor, heating to 140 DEG C, adding the phenyl dichlorophosphate or phenyl dibromophosphate, keeping the temperature for 1-2 hours, heating to 200-240 DEG C, and keeping the temperature for 2-4 hours, thereby obtaining a white solid flame retardant; and adding the white flame retardant into a solvent until the white flame retardant is completely dissolved, precipitating with 5-10 times of solvent amount of precipitating agent, filtering, and carrying out vacuum drying to obtain the white solid product. The ODOPB-base polyphosphate flame retardant has favorable compatibility with the polymeric matrix, can not easily transfer, and has excellent durability.

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 are viscous oily liquids, which are extremely inconvenient in the process of use, storage and transportation. At the same time, liquid flame retardants are easy to seep out of the matrix, resulting in a decrease in flame retardant performance. The flame retardant 10-(2,5-dihydroxyphenyl)-10-H-9-oxa-10-phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40C08L67/00C08L69/00C08L77/00C08L77/02C08L63/00C08L71/10
Inventor 班大明陈卓赵欧张永航刘真美韦万丽
Owner GUIZHOU NORMAL UNIVERSITY
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