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

A technology of caprolactone phosphate and flame retardant, which is applied in the field of phosphorus flame retardants, can solve the problems of not being able to meet the processing temperature of polymer materials, and achieve the effects of easy industrial production, high phosphorus content, and easy availability of raw materials

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of DOPO-containing dioxycaprolactophosphate flame retardant, the steps are:

[0025] Under nitrogen protection, add 12g DOPO (0.055mol) and 300mL toluene to the three-necked flask, heat and stir until DOPO is completely dissolved in toluene, add 5g p-benzoquinone (0.046mol), and stir the reaction at 100°C for 5h. The resulting precipitate was cooled to room temperature, filtered, reconstituted with methanol, and dried to obtain Intermediate I as a white solid.

[0026] 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 a yield of 91.2%.

[0027] In a round-bottomed flask with 100 mL of acetonitrile, add 3....

Embodiment 2

[0034] The solvent was changed to THF, and the others were the same as Example 1. The yield of the target compound was 85.1%, and the melting point was 233-235° C.

[0035] The solvent was replaced by DMF, and the others were the same as Example 1. The yield of the target compound was 83.2%, and the melting point was 233-235°C.

Embodiment 3

[0037] Increase the amount of intermediate II to 4.79 g (0.026 mol), and the others are the same as Example 1. The yield of the target compound is 90.5%, and the melting point is 233-235°C.

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Abstract

The invention discloses a DOPO-containing dioxacaprophosphate flame retardant. The flame retardant is prepared by the following steps: reacting DOPO and p-benzoquinone in an organic solvent 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 99.5 percent. The flame retardant can serve as a reactive flame retardant to be used in an epoxy resin, an ABS resin, polyurethane and other thermosetting resins, also can serve as an additive flame retardant, is used for meeting the halogen-free flame retardant requirements on ABS, nylon and other engineering plastics with high heat resistance requirements on the flame retardant and is wide in application prospects.

Description

technical field [0001] The DOPO-containing dioxycaprolactophosphate 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 dioxycaprolactophosphate flame retardant. It can be used as a reactive flame retardant to prepare a halogen-free flame retardant resin, and can also be used as an additive flame retardant for the halogen-free flame retardant of engineering plastics. Background technique [0002] Polymer materials are widely used in various sectors of the national economy such as industry, agriculture, and military, but most polymers are petroleum-based combustible materials, which have high heat release rate, large calorific value, fast flame propagation speed and are not easy to burn. If it is extinguished, thick smoke and toxic gas will generally be produced, which poses a huge threat to people's life and property safety. When traditional haloge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C07F9/6574C08L63/00C08L75/04C08L55/02
Inventor 李德江刘义稳谢益碧
Owner CHINA THREE GORGES UNIV
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