Alkylphosphinate derivative fire retardant containing phosphaphenanthrene group and preparation method thereof

A technology of alkyl phosphinate and derivatives, applied in the field of alkyl phosphinate derivative flame retardants and their preparation, can solve problems such as unreported

Active Publication Date: 2017-03-29
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In this application, by introducing a special bridge structure to bond phosphaphenanthrene and alkyl phosphinate into the same molecular structure, a new type of alkyl phosphinate derivative containing phosphaphenanthrene group is constructed. flame retardants, which have not been reported in the literature and published materials

Method used

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  • Alkylphosphinate derivative fire retardant containing phosphaphenanthrene group and preparation method thereof
  • Alkylphosphinate derivative fire retardant containing phosphaphenanthrene group and preparation method thereof
  • Alkylphosphinate derivative fire retardant containing phosphaphenanthrene group and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 84.11g (0.20mol) of o-diallyl bisphenol A diglycidyl ether and 86.47g (0.40mol) of DOPO into the reaction vessel, raise the temperature of the reaction system to 160°C under stirring conditions, and react at constant temperature for 6 hours Afterwards, the reaction was terminated, and the molten fluid reaction product flowed out of the reaction vessel, and cooled to room temperature to form a light yellow glassy transparent solid, which was the primary intermediate ABD, and its infrared spectrum was as attached figure 1 As shown, the thermogravimetric curve is attached figure 2 shown.

[0036] Take 85.29g (0.10mol) of primary intermediate ABD and 31.68g (0.24mol) of 50wt.% hypophosphorous acid aqueous solution into a reaction vessel containing 500mL of propanol, heat up to 65°C, and stir until the reactants are completely After dissolving, add 9.85g (0.06mol) azobisisobutyronitrile initiator, stir and react at a constant temperature for 48 hours to obtain the seco...

Embodiment 2

[0038] Add 42.05g (0.10mol) of o-diallyl bisphenol A diglycidyl ether, 64.85g (0.30mol) of DOPO and 100mL of dichlorobenzene into the reaction vessel, and raise the temperature of the reaction system to 170°C while stirring. After stirring the reaction at constant temperature for 8 hours, the reaction was terminated, and the solvent dichlorobenzene was distilled off under reduced pressure, and the molten liquid reaction product was flowed out of the reaction vessel, and cooled to room temperature to form a light yellow glassy transparent solid, which was the primary intermediate Body ABD.

[0039] Take 85.29g (0.10mol) of primary intermediate ABD and 7.92g (0.12mol) of anhydrous hypophosphorous acid into a reaction vessel filled with 400mL of ethanol, raise the temperature to 66°C, stir well until the reactants are completely dissolved, then add 3.45 g (0.015mol) dimethyl azobisisobutyrate initiator, stirred and reacted at a constant temperature for 36 hours to obtain the seco...

Embodiment 3

[0041] Add 84.11g (0.20mol) of o-diallyl bisphenol A diglycidyl ether, 86.47g (0.40mol) of DOPO and 150mL of xylene into the reaction vessel, and raise the temperature of the reaction system to 145°C under stirring conditions, and keep the temperature constant After stirring the reaction for 10 hours, the reaction was terminated, and the solvent xylene was removed by distillation under reduced pressure, and the molten liquid reaction product flowed out of the reaction vessel, and cooled to room temperature to form a light yellow glassy transparent solid, which was the primary intermediate ABD .

[0042] Take 85.29g (0.10mol) of primary intermediate ABD and 19.36g (0.22mol) of sodium hypophosphite into a reaction vessel containing 600mL of ethanol, raise the temperature to 71°C, stir well until the reactants are completely dissolved, then add 19.38g (0.08mol) dibenzoyl peroxide initiator, after constant temperature stirring reaction for 45 hours, the secondary intermediate ABDP...

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Abstract

The invention discloses an alkylphosphinate derivative fire retardant containing a phosphaphenanthrene group. A preparation method of the fire retardant is as follows: fusion or solution system addition reaction is carried out for P-H bonds on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and epoxide groups and C=C double bonds on o-diallyl bisphenol A diglycidyl ether, in order to obtain a primary intermediate ABD; an addition reaction is carried out between hypophosphorous acid and / or P-H bond on salt thereof and residual C=C double bonds of the primary intermediate ABD initiated by free radicals, in order to obtain a secondary intermediate ABDP and / or salts thereof; metallic compounds and / or protonated nitrogen base are added, an alkaline substance is added for neutralization of acids in the reaction system, a target material is salified and separated, and alkylphosphinate M-ABDP containing the phosphaphenanthrene group is prepared. The M-ABDP has good application prospects, and can be widely applied to flame retardation modification of polyester, polyamide and thermosetting resin, and other high-molecular resin materials.

Description

technical field [0001] The invention relates to an alkyl phosphinate derivative flame retardant containing a phosphaphenanthrene group and a preparation method thereof, and belongs to the technical field of preparing flame retardant materials by chemical synthesis methods. Background technique [0002] Alkyl phosphinate is a phosphorus-based flame retardant first commercialized by Clariant Company in Germany. It has good hydrophobicity and thermal stability, and is currently widely used in polyester (CN200980137336.X), polyamide ( In polymer resin materials such as CN201110223494.6) and thermosetting materials (CN201510445555.1), excellent flame retardant properties can be endowed to the resin material, and the flame retardant modified resin material of the alkyl phosphinate is superior in processing performance, physical and mechanical properties , electrical performance and smoke generation performance are all good. [0003] 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-ox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5313
CPCC07F9/657172C08K5/5313
Inventor 钱立军邱勇陈雅君
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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