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DOPO-based flame retardant, and preparation method thereof

A technology of flame retardant and solvent, which is applied in the field of DOPO-based flame retardant and its preparation, can solve the problems of large amount of flame retardant added, achieve good flame retardant effect, improve flame retardant performance, high purity and high yield Effect

Active Publication Date: 2016-12-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant material can only reach the V-0 level when the amount of flame retardant added is 50wt%, and the amount of flame retardant added is relatively large.

Method used

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  • DOPO-based flame retardant, and preparation method thereof
  • DOPO-based flame retardant, and preparation method thereof
  • DOPO-based flame retardant, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044]In the first step, add 0.5mol (108g) DOPO (9,10-di Hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide) and 200mL toluene, stirred and heated to 80°C under nitrogen protection, after stirring until DOPO was completely dissolved, added 15g of paraformaldehyde, and then heated to Reflux reaction at 95°C for 8 hours, white precipitate will be produced during the reaction. When the reaction was complete, the reaction was stopped, and the precipitate was filtered and washed with toluene and vacuum-dried at 70° C. for 10 h to obtain dry product I.

[0045] In the second step, phenyl dichlorinated phosphate (PDCP) (21.1g, 0.1mol) and 80mL tetrahydrofuran (THF) were added into a 250mL three-necked flask equipped with a mechanical stirrer, and the temperature of the system was controlled at 0°C; Triethylamine (TEA) (21.3g, 0.21mol) was added to the system; then hydroxyethyl acrylate (HEA) (11.6g, 0.1mol) and 20mL THF were added dropwise, and the process continued for 2 hours; after t...

Embodiment 2

[0049] In the first step, add 0.5mol (108g) DOPO and 200mL toluene to a 500mL three-necked flask equipped with a thermometer, a nitrogen inlet tube and a reflux condenser (the tail end is connected to an anhydrous calcium chloride drying tube), and the Under protection, stir and heat up to 75°C. After stirring until DOPO is completely dissolved, add 15g of paraformaldehyde, then heat up to 90°C and reflux for 10 hours. White precipitate will appear during the reaction. When the reaction was complete, the reaction was stopped, and the precipitate was filtered and washed with toluene and vacuum-dried at 80° C. for 10 h to obtain dry product I.

[0050] In the second step, phenyl dichlorinated phosphate (PDCP) (21.1g, 0.1mol) and 80mL of dichloromethane were added into a 250mL three-necked flask equipped with a mechanical stirrer, and the temperature of the system was controlled at -10°C; Add triethylamine (TEA) (21.3g, 0.21mol) in the system; Then drop into hydroxyethyl methacry...

Embodiment 3

[0054] In the first step, add 0.5mol (108g) DOPO and 200mL toluene to a 500mL three-necked flask equipped with a thermometer, a nitrogen inlet tube and a reflux condenser (the tail end is connected to an anhydrous calcium chloride drying tube), and the Under protection, stir and heat up to 80°C. After stirring until DOPO is completely dissolved, add 15g of paraformaldehyde, then heat up to 95°C and reflux for 8 hours. White precipitate will appear during the reaction. When the reaction was complete, the reaction was stopped, and the precipitate was filtered and washed with toluene and vacuum-dried at 70° C. for 12 h to obtain dry product I.

[0055] In the second step, add phenyl dichlorinated phosphate (PDCP) (21.1g, 0.1mol) and 80mL chloroform into a 250mL three-necked flask equipped with a mechanical stirrer, and control the temperature of the system at 5°C; after 30 minutes, add Triethylamine (TEA) (21.3g, 0.21mol); Add hydroxyethyl acrylate (HEA) (11.6g, 0.1mol) and 20mL ...

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Abstract

The invention discloses a DOPO-based flame retardant, and a preparation method thereof. According to the preparation method, 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide and paraformaldehyde are taken as raw materials, and a precursor I is synthesized via substitution reaction; active hydroxide radicals of the precursor I, phenyl dichlorophosphate, and hydroxyethyl acrylate are subjected to substitution / esterification reaction so as to prepare a flame retardant which is high in phosphorus content and possesses active double bonds; and the flame retardant is added into an unsaturated polyester resin matrix so as to obtain a flame-retardant unsaturated polyester resin composite material. According to the DOPO-based flame retardant, flame resistance of the unsaturated polyester resin matrix is improved via a gas phase and a condensed phase, problems of conventional additive flame retardants that compatibility with polymer matrix is poor, migration is easily caused, and flame retardant efficiency is low are solved. When the DOPO-based flame retardant is applied to inflaming retarding of unsaturated polyester resin, material vertical flame rating is capable of reaching V-0 grade at a relatively low adding amount, and flame resistance is excellent. The DOPO-based flame retardant is high in purity and yield, and aftertreatment is simple.

Description

technical field [0001] The invention belongs to the technical field of flame retardant design and preparation, and in particular relates to a DOPO-based flame retardant and a preparation method thereof. Background technique [0002] Due to many excellent properties such as good chemical stability, easy processing, and low cost, polymer materials have been widely used in many fields such as electronic communications, biomedicine, aerospace, automobile industry, and construction. However, most polymer materials are easy to decompose and burn at high temperatures, and release a lot of heat and toxic gases at the same time, endangering human life and property safety. In order to realize the full potential of these polymer materials in industrial applications, it has become necessary to improve their flame retardancy. At present, it is widely used to add flame retardants to various polymers to improve their flame retardant properties. Phosphorus-containing flame retardants have ...

Claims

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Application Information

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IPC IPC(8): C08K5/5373C08K5/5313C08L67/06C08L63/10C07F9/6574
CPCC07F9/65744C08K5/5313C08K5/5373C08L2201/02C08L67/06C08L63/10
Inventor 江赛华师星星
Owner SOUTH CHINA UNIV OF TECH
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