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Preparation method and application of spiro-phosphate flame retardant containing DOPO and benzoxazine

A technology of spirocyclic phosphate and benzoxazine, which is applied in the field of phosphorus-nitrogen synergistic flame retardant compounds, can solve the problem of high price of spirocyclic phosphate, and achieve the effects of good thermal stability, high phosphorus content and high flame retardant rate

Inactive Publication Date: 2018-09-28
CHINA THREE GORGES UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the weak point in the above-mentioned prior art, provide a kind of technique simple, production cost is low, overcome the shortcoming that spirocyclic phosphate price is high, synthesize intermediate II (spirophosphoric acid ester) by reaction of phosphorus oxychloride and pentaerythritol Cyclic phosphate dichloride), use 4-aminophenol, 2-hydroxybenzaldehyde, DOPO, formaldehyde to synthesize intermediate I, intermediate I and intermediate II react to form a new type of DOPO and benzoxazine with excellent flame retardancy spirocyclic phosphate flame retardant

Method used

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  • Preparation method and application of spiro-phosphate flame retardant containing DOPO and benzoxazine
  • Preparation method and application of spiro-phosphate flame retardant containing DOPO and benzoxazine

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Embodiment 1

[0031] A preparation method of a spirocyclic phosphate flame retardant containing DOPO and benzoxazine, the steps are:

[0032] Add 13.10 g (0.12 mol) of 4-aminophenol, 14.66 g (0.12 mol) of 2-hydroxybenzaldehyde, 25.94 g (0.12 mol) of DOPO, and 250 mL of methanol into a flask equipped with a stirrer, a reflux condenser and a tail gas absorber. Nitrogen gas was introduced, and after 10 hours of reaction at room temperature, 9.84 g (0.12 mol) of 37% formaldehyde was added, and the reaction was carried out at room temperature for 6 hours. After the reaction, the reaction solution was poured into 300 mL of water, and a large amount of white solid was precipitated, which was filtered by suction and dried in vacuum to obtain Intermediate I with a yield of 91.2%.

[0033] Add 27.24g (0.20mol) of pentaerythritol, 300mL of acetonitrile and 91.2g (0.60mol) of phosphorus oxychloride (POCl 3 ), react at 75°C-80°C for 12h, until no hydrogen chloride gas is generated; cool to room tempera...

Embodiment 2

[0043] The solvent was changed to N, N-dimethylacetamide, and the others were the same as Example 1, and the yield of the target compound was 80.5%.

[0044]The solvent was changed to dimethyl sulfoxide, and the others were the same as Example 1, and the yield of the target compound was 81.7%.

Embodiment 3

[0046] The acid-binding agent triethylamine was replaced by N,N-dimethylaniline, and the others were the same as Example 1, and the yield of the target compound was 83.6%.

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Abstract

The invention relates to a preparation method and application of a spiro-phosphate flame retardant containing DOPO and benzoxazine. An intermediate I is synthesized by using 4-aminophenol, 2-hydroxybenzaldehyde, DOPO and formaldehyde through a one-pot method under the action of methanol; a second intermediate II (spiro-phosphate oxalyl chloride) is synthesized by using phosphorus oxychloride and pentaerythritol; and the spiro-phosphate flame retardant containing DOPO and benzoxazine and having the appearance of white solid powder is obtained through the reaction of the intermediate I and the intermediate II. The flame retardant has an initial decomposition temperature of about 320 DEG C, the weight loss reaches 9% at 450 DEG C, and the char yield of the flame retardant at 700 DEG C reaches58%. The flame retardant has good thermal stability, high char yield and good flame-retardant effect, and can be used for halogen-free flame retardance of the polypropylene and acrylonitrile butadiene styrene (ABS).

Description

technical field [0001] The invention belongs to the technical field of phosphorus-nitrogen synergistic flame-retardant compounds, and specifically relates to a spirocyclic phosphate flame retardant containing DOPO and benzoxazine. The flame retardant has good thermal stability, high carbon residue rate, Good flame retardant effect, can be used for non-halogen flame retardant of polypropylene and ABS. Background technique [0002] Halogenated flame retardants are flame retardant polymers that produce hydrogen halides and other corrosive and toxic thermal cracking products when burned. As people's awareness of environmental protection continues to increase, halogen-free flame retardants have become an inevitable trend in the development of flame retardants. DOPO is a new type of flame retardant intermediate. Its structure contains active phosphorus-hydrogen bonds. It is very active to olefins, epoxy bonds and carbonyl groups, and can react to produce many derivatives. Due to ...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C08L23/12C08L55/02C07F9/6574C07F9/6571
Inventor 李德江鄢柳柳杨香萍邹德荣
Owner CHINA THREE GORGES UNIV
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