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Polyphosphamide fire retardant with bicyclic phosphate structure and preparation method thereof

A technology of bicyclic phosphate and polyphosphoramid, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of small molecular weight, poor compatibility, easy moisture absorption, etc. Achieve the effect of high carbon formation rate, good thermal stability and high content

Inactive Publication Date: 2014-05-14
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to fundamentally overcome the problems of small molecular weight, easy moisture absorption, poor compatibility, easy migration and low-molecular phosphate flame retardants existing in traditional multi-component compounded intumescent flame retardants. Does not contain the problem of gas source nitrogen, design and synthesize a polymeric intumescent flame retardant containing acid source, carbon source, and gas source as a whole, containing a variety of flame retardant elements, good thermal stability, and high char formation rate

Method used

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  • Polyphosphamide fire retardant with bicyclic phosphate structure and preparation method thereof
  • Polyphosphamide fire retardant with bicyclic phosphate structure and preparation method thereof
  • Polyphosphamide fire retardant with bicyclic phosphate structure and preparation method thereof

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Experimental program
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Embodiment 1

[0028] Step 1: Under nitrogen protection, add 3.06g (0.020mol) of phosphorus oxychloride, 3.60g (0.020mol) of PEPA, and 30ml of dioxane into a four-necked flask equipped with a stirrer, reflux condenser, and thermometer. Continue to stir for 30 minutes to disperse PEPA evenly, then raise the temperature to 70°C for 5 hours, cool to room temperature after the reaction, and obtain a solution containing the intermediate PEPA dichlorophosphate;

[0029] Step 2: Add 30 ml of dioxane solution containing 4.96 g (0.020 mol) of 4,4′-diaminodiphenylsulfone and 1.58 g of pyridine (0.020 mol) to the intermediate dichlorophosphate PEPA obtained in step 1 In the ester solution, under stirring conditions, first react at 70°C for 1h, then heat up to 100°C for 8h, cool to room temperature after the reaction, filter to obtain 8.27g of crude product, wash with water, wash with ethanol two-step purification process, after purification After drying at 60°C, 7.07 g of white fluffy powder was obtain...

Embodiment 2

[0035]Step 1: Under nitrogen protection, add 3.82g (0.025mol) of phosphorus oxychloride, 3.60g (0.020mol) of PEPA, 1-methyl-2 - 50ml of pyrrolidone, continue stirring for 30min to disperse PEPA evenly, then raise the temperature to 60°C for 6h, cool to room temperature after the reaction, and obtain a solution containing the intermediate PEPA dichlorophosphate;

[0036] Step 2: Add 50 ml of 1-methyl-2-pyrrolidone solution containing 5.21 g (0.021 mol) of 4,4′-diaminodiphenylsulfone and 2.22 g of triethylamine (0.022 mol) to the intermediate-containing In a solution of PEPA dichlorophosphate, under stirring conditions, first react at 65°C for 2h, then raise the temperature to 120°C for 6h, cool to room temperature after the reaction, filter to obtain 9.27g of crude product, wash with water and wash with acetone for two steps Purification process, drying at 80°C after purification to obtain 7.87g of white fluffy powder, which is a polyphosphoramide flame retardant containing a b...

Embodiment 3

[0038] Step 1: Under nitrogen protection, add 3.37g (0.022mol) of phosphorus oxychloride, 3.60g (0.020mol) of PEPA, and 30ml of acetonitrile into a four-neck flask equipped with a stirrer, reflux condenser, and thermometer, and continue stirring for 30min to disperse PEPA evenly, then raise the temperature to 60°C for 6 hours, and cool to room temperature after the reaction to obtain a solution containing the intermediate PEPA dichlorophosphate;

[0039] Step 2: Add 50 ml of acetonitrile solution containing 6.20 g (0.025 mol) of 4,4′-diaminodiphenylsulfone and 2.53 g of triethylamine (0.025 mol) to the PEPA containing intermediate dichlorophosphate obtained in step 1 In the solution, under stirring conditions, first react at 60°C for 2h, then heat up to 80°C for 12h, cool to room temperature after the reaction, filter to obtain 9.57g of crude product, wash with water, wash with ethanol two-step purification process, after purification 60 ℃ drying to obtain 8.49 g of white fluf...

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Abstract

The invention relates to a polyphosphamide fire retardant with a bicyclic phosphate structure and a preparation method thereof. The structural formula of the polyphosphamide fire retardant is shown in the specification, wherein n is an integer between 2 and 2000. The preparation method of the polyphosphamide fire retardant comprises the following steps of: carrying out substitution reaction between phosphorus oxychloride and 1-oxo-4-hydroxymethyl-2,6,7-trioxo-1-phosphabicyclo[2,2,2] octane (PEPA) to prepare an intermediate, then carrying out polycondensation on the intermediate and 4, 4'-diamino diphenyl sulfone under the action of an acid-binding agent to obtain the final product. Because of containing three flame-retardant elements, namely phosphorus, nitrogen and sulphur, the polyphosphamide fire retardant disclosed by the invention solves the problem that a multicomponent intumescent flame retardant is single in flame-retardant element variety, is not uniformly distributed in a material and excessively consumes mechanical property when added in a large quantity; and the polyphosphamide fire retardant has the advantages of high initial thermal decomposition temperature, good thermal stability and high char yield at a high temperature and can be applied to the flame-retardant modification of materials such as polyamide and polyester, independently or in a compound manner.

Description

technical field [0001] The invention relates to a polyphosphoramide flame retardant containing a bicyclic phosphate structure and a preparation method thereof, belonging to the technical field of preparation of polymeric flame retardants. Background technique [0002] The extensive application of polymer materials in social life not only brings convenience to people's lives, but also brings fire hazards to people. Adding flame retardants is one of the most effective ways to reduce the ignition performance of polymer materials. Intumescent flame retardants have been widely used and favored by researchers for their low toxicity, halogen-free and unique char formation flame retardant mechanism. However, the chemical substances used as the three components of carbon source, acid source and gas source in traditional intumescent flame retardants are often small molecules, which contain a single flame retardant element and need to be used in multiple compounds, and the molecular w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/02C07F9/6574
Inventor 刘吉平赵伟
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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