Polyphosphate oligomer flame retardant and preparation method thereof

A polyphosphate and oligomer technology, applied in the field of polyphosphate oligomer and phosphate oligomer flame retardant, can solve the problems of increasing process complexity and difficulty, and achieve efficient preparation, low volatile content and less , the effect of good product quality

Active Publication Date: 2016-12-07
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to reduce low-volatility polyphosphates and reduce by-products, it is necessary to remove excess POCl through related procedures. 3 , which will inevitably increase the complexity and difficulty of the target product preparation process

Method used

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  • Polyphosphate oligomer flame retardant and preparation method thereof
  • Polyphosphate oligomer flame retardant and preparation method thereof
  • Polyphosphate oligomer flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 456g (2mol) of bisphenol A (BPA), 378g (2.13mol) of diethyl nitrile methyl phosphate, and 4.2g (0.5%) of catalyst NaOH into a multi-necked flask equipped with a stirrer and nitrogen inlet and outlet. After replacing the air, pass nitrogen protection, gradually increase the temperature, and start stirring after the BPA melts. The temperature is gradually raised from 140°C to 200°C. At the same time, the pressure is gradually reduced from 760mmHg to the final residual pressure of 10mmHg. The entire reaction process takes 3.5 to 5 hours. The step-by-step temperature rise and negative pressure are controlled as follows:

[0038] 140°C×1.5h×760mmHg, 160°C×1h×200mmHg, 180°C×0.5h×50mmHg, 200°C×0.5h×10mmHg, after the reaction, a light brown viscous liquid was obtained with a yield of 90%. The viscosity of the product was measured as 820mPa.

[0039] Infrared Spectrum ( figure 1 ) shows that at 2258cm -1 Nitrile characteristic absorption appears at 1246cm -1 The left and...

Embodiment 2

[0041] Using tetrabutylphosphine hydroxide and NaOH as the composite catalyst (the weight ratio of the two is 1:1), the amount of catalyst added is 0.3% (2.5g) of the total weight of 456g of bisphenol A (BPA) and 378g of diethyl nitrile methyl phosphate , other with embodiment 1. After the reaction was finished, the polyphosphate oligomer of light brown viscous liquid was obtained, the yield was 92%, and the measured product viscosity was 850mPa.

Embodiment 3

[0043] Lanthanum acetylacetonate was used as the catalyst, and the amount of the catalyst added was 0.3% (2.5 g) of the total weight of 456 g of bisphenol A (BPA) and 378 g of diethyl nitrile methyl phosphate. Others were the same as in Example 1. After the reaction was finished, a polyphosphate oligomer of light brown viscous liquid was obtained, the yield was 89%, and the measured product viscosity was 780mPa.

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Abstract

The invention provides a polyphosphate oligomer flame retardant represented as the formula (I) and preparation method thereof, wherein R refers to a C1-C5 alkylene group, e.g., a methylene group; X refers to a bisphenol structure unit, which can be bisphenol A, diphenol, bisphenol AF, bisphenol S, bisphenol fluorene, resorcinol and the like; n is a positive integer from 2 to 20. The preparation method includes the steps of: under a catalytic condition of a catalyst, performing a bulk polymerization reaction to a phosphate monomer (II) and a bisphenol monomer, wherein alcohol or phenol removal occurs in the process and the reaction is free of HCl escape. The production is high in contents of both phosphorus and nitrogen and is low in low-volatile ingredient. The method is simple, is short in reaction time, is low in environment pollution and is easy to achieve in industrial production.

Description

technical field [0001] The invention relates to a polyphosphate oligomer, in particular to a kind of phosphate oligomer flame retardant with a nitrile structural unit, and a preparation method thereof, belonging to the technical field of polymer flame retardant materials. Background technique [0002] Polyphosphate oligomers are a class of flame retardants that have recently been vigorously developed, and their preparation is usually made of phosphorus oxychloride (POCl 3 ), phosphorus trichloride, arylphosphonyl halide (such as phenylphosphonyl dichloride), or phosphorus oxychloride reacts with phenol to form an intermediate (such as bisphenol tetrachlorobisphosphate, diarylphosphoryl chloride) as Phosphorus-containing starting materials are then prepared by reacting with bisphenols and / or phenols. Related patent applications are as follows: [0003] 1) The patent application number 2006101663106, the patent titled "Preparation method of oligomeric phosphate or oligomeric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C07F9/40C08K5/521
CPCC07F9/4046C08G79/04C08K5/521
Inventor 邓清田唐培徐亭宋升吴勇周楠
Owner CHINA BLUESTAR CHENGRAND CO LTD
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