No-halogen fire-proof phosphorus-containing compound with high heat stability and its prepn

A high thermal stability, compound technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as use restrictions, insufficient thermal stability, etc. The effect of strong resistance, high phosphorus content and thermal stability

Active Publication Date: 2007-01-03
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] DOPO is mainly introduced into the polymer as a reactive monomer, which can obtain a good flame retardant effect, but as an additive flame retardant such as nylon, its thermal stability is not enough and its use is limited

Method used

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  • No-halogen fire-proof phosphorus-containing compound with high heat stability and its prepn
  • No-halogen fire-proof phosphorus-containing compound with high heat stability and its prepn
  • No-halogen fire-proof phosphorus-containing compound with high heat stability and its prepn

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a four-necked round-bottomed flask equipped with a nitrogen inlet, a condenser and a thermometer, add a solution of DOPO (compound 1) in dimethylformamide, pass nitrogen, control the temperature at 90 ° C, and drop the equivalent of The dimethylformamide solution of diphenylmethane bismaleimide (compound 2) with half the number of DOPO moles (that is: the molar ratio of compound 1: compound 2 is 2: 1), the dropwise process temperature is controlled at Around 90°C. After the dropwise addition, the temperature rose to 110°C. After two hours of reaction, the reaction was stopped, washed with ethanol, and dried in vacuum at 80°C to obtain a white solid substance with a melting point of 233°C——DOPO derivative A.

Embodiment 2

[0038] In a four-necked round-bottomed flask equipped with a nitrogen inlet, condenser and thermometer, add diphenylmethane bismaleimide (compound 2) and DOPO twice its molar number, nitrogen, and the reaction mixture is heated to 180°C, temperature controlled and reacted for 4 hours. After the reaction was completed, a quantitative amount of xylene was added. Stir and filter. The obtained solid was washed twice with xylene, and dried under vacuum at 100°C to obtain a white solid with a melting point of 233°C——DOPO derivative A.

Embodiment 3

[0040] In a four-neck round-bottomed flask equipped with a nitrogen inlet, a condenser and a thermometer, add a solution of DOPO in dimethylformamide, pass nitrogen, control the temperature at 90°C, and add a solution equivalent to the number of moles of DOPO dropwise within two hours. Half of the dimethylformamide solution of benzophenone bismaleimide (compound 2), the temperature of the dropping process is controlled at about 90°C. After the dropwise addition, the temperature rose to 110°C. After two hours of reaction, the reaction was stopped, washed with ethanol three times, and dried in vacuum at 80°C to obtain a white solid substance——DOPO derivative B.

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Abstract

The present invention is no-halogen fireproof phosphorus-containing compound with high heat stability and its preparation process, and features that the phosphorus-containing compound is prepared with 9, 10-dihydro-9-oxa-10-phospha phenanthryl-10-oxide, bismaleimide and other material and through solution process or fusion process. This kind of the phosphorus-containing compound has high heat stability and high antiflaming efficiency, and may be used as flame retardant for preparing no-halogen fireproof resin. Its chemical structure is shown.

Description

technical field [0001] The invention belongs to phosphorus compounds, and relates to a halogen-free flame-retardant phosphorus-containing compound with high thermal stability and a preparation method thereof. This type of phosphorus-containing compound has high heat resistance and flame-retardant efficiency, and can be used as a flame retardant to prepare halogen-free flame-retardant Burn resin. Background technique [0002] At present, organophosphorus heterocyclic compounds are a research hotspot in organophosphorus chemistry, and they are also one of the more active fields in recent flame retardant research. Organophosphorous heterocyclic compound flame retardants mainly include five-membered rings, six-membered rings and spiro ring compounds. Among them, phosphorus-containing six-membered ring compounds are dominant. In recent years, the synthesis and application of flame retardants with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (hereinafter referred to as DOP...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571C09K21/12C08K5/53
Inventor 吴俊涛唐超王德生唐安斌杨士勇
Owner SICHUAN DONGFANG INSULATING MATERIAL
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