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DOPO-containing cyclic phosphate flame retardant as well as preparation method and application thereof

A technology of cyclic phosphate ester and bicyclic phosphate ester, which is used in the preparation of halogen-free flame retardants, dioxycaprolactone phosphate flame retardants, and cyclic phosphate esters. It can solve problems such as the inability to meet the processing temperature of polymer materials. Achieve the effects of easy industrial production, easy access to raw materials, and good thermal stability

Inactive Publication Date: 2015-04-29
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the direct use of DOPO monomer for flame retardancy of polymer materials has the disadvantage that it begins to decompose at 180°C, which cannot meet the processing temperature of most polymer materials.

Method used

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  • DOPO-containing cyclic phosphate flame retardant as well as preparation method and application thereof
  • DOPO-containing cyclic phosphate flame retardant as well as preparation method and application thereof
  • DOPO-containing cyclic phosphate flame retardant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of a DOPO-containing dioxycaprolactophosphate flame retardant, the steps are:

[0024] Into the three-necked flask under the protection of nitrogen, add 4,4 / - 21.4 g (0.10 mol) of dihydroxybenzophenone and 43.2 g of DOPO (0.20 mol) were heated and stirred to 200° C., and stirred for 5 hours. After the reaction was completed, the resulting precipitate was cooled to room temperature and filtered, and was washed with THF-Et 2 O(V THF :V Et2O =7:3) The heavy product was dried to obtain Intermediate I, a white powdery solid, with a yield of 79.5%.

[0025] Add 52.0g (0.5mol) of neopentyl glycol and 200mL of chloroform into the flask, slowly add 84.3g (0.55mol) of phosphorus oxychloride dropwise under stirring, and react at 65°C for 6h after the dropwise addition. After the reaction was completed, chloroform and excess phosphorus oxychloride were distilled off to obtain a white solid, which was recrystallized and dried to obtain intermediate II with...

Embodiment 2

[0033] The solvent in step C was replaced by THF, and the others were the same as Example 1. The yield of the target compound was 82.5%, and the melting point was 282-284°C.

Embodiment 3

[0035] In step C, the solvent was changed to DMAC, and the others were the same as Example 1. The yield of the target compound was 84.3%, and the melting point was 233-235°C.

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Abstract

The invention discloses a DOPO-containing cyclic phosphate flame retardant. The flame retardant is prepared by the following steps: reacting 4,4 / -dihydroxy benaophenonel and DOPO so as to obtain an intermediate I; preparing an intermediate II from neopentyl glycol and phosphorus oxychloride under the action of chloroform; and reacting the intermediate I and the intermediate II in an organic solvent, thereby obtaining the flame retardant. The flame retardant is white in appearance, high in thermal stability and high in flame retardant rate and has the purity of 98.6 percent. According to the flame retardant, the DOPO, benzophenone oxygroup structural units are introduced into the phosphate, and the flame retardant has high phosphorus content, high heat resistance and high-temperature char yield, can serve as a reactive flame retardant, also can serve as an additive flame retardant and is wide in application prospects.

Description

technical field [0001] The cyclic phosphate ester containing double DOPO of the present invention belongs to the technical field of phosphorus-based flame retardants, and specifically relates to a preparation method and application of a DOPO-containing dioxycaprolactone phosphate flame retardant. The flame retardant can be used as a reactive type The flame retardant is used to prepare halogen-free flame-retardant resins, and can also be used as an additive flame retardant for halogen-free flame retardants in engineering plastics. Background technique [0002] Phosphate ester flame retardants have the advantages of low smoke, non-toxic, halogen-free, good compatibility with materials, long-lasting flame retardant effect, water resistance, heat resistance, migration resistance, etc., and play a role in flame retardancy and plasticization in polymer materials role, has good development prospects. Especially cyclic phosphate flame retardants, because they contain a six-membered...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C07F9/6574C08L69/00C08L55/02
Inventor 李德江刘义稳谢益碧
Owner CHINA THREE GORGES UNIV
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