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Phosphorus-nitrogen quaternary ammonium as well as preparation method and application thereof

A quaternary ammonium salt, phosphorus nitrogen technology, applied in chemical instruments and methods, dyed low molecular organic compound treatment, organic chemistry, etc. and other problems, to solve the migration problem, increase the flame retardant performance, and reduce the amount of use

Inactive Publication Date: 2011-11-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the organically treated montmorillonite can be well dispersed in the polymer, the intercalation agent used is often a long carbon chain organic cationic compound (such as hexadecyl triethylene oxide) with poor thermal stability and no flame retardant effect. methylammonium bromide), thus affecting the flame retardancy of polymer / montmorillonite nanocomposites

Method used

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  • Phosphorus-nitrogen quaternary ammonium as well as preparation method and application thereof
  • Phosphorus-nitrogen quaternary ammonium as well as preparation method and application thereof
  • Phosphorus-nitrogen quaternary ammonium as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Example 1: Synthesis of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine

[0042] Add 15.4g (0.1mol) of phosphorus oxychloride and 50mL of chloroform into a four-necked flask, stir the reaction temperature to 35°C, slowly add dropwise a mixture of 10.4g (0.1mol) of neopentyl glycol and 80mL of chloroform, After the addition, the reaction was maintained at 40°C for 3 hours, the chloroform was recovered by distillation under reduced pressure, washed with 25 mL of anhydrous ether, and filtered to obtain a colorless crystalline solid of 2-oxo-2-chloro-5,5-dimethyl -1,3,2-Dioxaphosphorinane, the yield is 86.1%, the purity is 97.1%, and the melting point is 109-110°C. Add 9.0g (0.15mol) of ethylenediamine and 40mL of chloroform into the three-necked flask, stir, and the temperature of the reaction solution is 0°C, slowly add 18.4g (0.1mol) of the solid (2-oxo-2 -Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane) and 100mL chloroform mixture, after the addition, keep the...

Embodiment 2

[0044] The synthesis operation of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine is the same as in Example 1. In the reaction of the formula (II) compound and the formula (III) compound, the amount ratio of the feed material of the formula (II) compound and the formula (III) compound is 1.0: 3.0, the solvent is selected diethyl ether, the reaction temperature is -30 ℃, and the reaction time is After 5 hours, the yield was 45.4%.

Embodiment 3

[0046] The synthesis operation of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine is the same as in Example 1. In the reaction of the formula (II) compound and the formula (III) compound, the amount ratio of the feed material of the formula (II) compound and the formula (III) compound is 1.0: 2.5, the solvent is selected diethyl ether, the reaction temperature is -20 ℃, and the reaction time is After 7 hours, the yield was 65.4%.

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Abstract

The invention discloses a phosphorus-nitrogen quaternary ammonium as well as a preparation method and application thereof. The phosphorus-nitrogen quaternary ammonium has a structure shown in the formula (I) and is prepared by the following steps: volution-contained phosphoryl chloride shown in the formula (II) is reacted with diamine compound shown in the formula (III) to obtain a compound shownin the formula (IV); the compound shown in the formula (IV) is reacted with acyl halide shown in the formula (V) to obtain a compound shown in the formula (VI); and the compound shown in the formula (VI) is reacted with tertiary amine shown in the formula (VII) to obtain the product, i.e. the phosphorus-nitrogen quaternary ammonium. The invention is used for chemically modifying montmrillonoid byusing the phosphorus-nitrogen quaternary ammonium, improves the inflaming retarding effect to high polymer materials through the cooperative inflaming retarding function of the montmrillonoid and phosphorus-nitrogen fire retardant, reduces the consumption of the fire retardant in the high polymer materials and lowers the cost of fire-retarding materials.

Description

(1) Technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a phosphorus-nitrogen type quaternary ammonium salt and its preparation method and application, especially its application in the preparation of a composite organophosphorus-nitrogen series-montmorillonite flame retardant. (2) Background technology [0002] Polymer / montmorillonite nanocomposites have unique flame retardant properties. Compared with traditional flame retardant materials, they have the characteristics of small addition, halogen-free, and small impact on the properties of matrix materials. It is one of the important directions for the development of flame retardant technology. . However, polymer / montmorillonite nanocomposites cannot meet the requirements of general materials for flame retardancy. In order to maximize the flame retardancy of polymer materials, the existing technology often uses montmorillonite and organic flame retardants. fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6571C09K21/12C09C3/08C09C1/42C08K9/04
Inventor 黄国波高建荣贾建洪李郁锦盛卫坚韩亮
Owner ZHEJIANG UNIV OF TECH
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