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Method for preparing retardant resorcin phosphate

A technology of resorcinol phosphate and resorcinol, which is applied in the field of preparation of halogen-free phosphate flame retardants, can solve the problems of harsh reaction conditions, difficulty in industrialization, and high equipment requirements, and achieve a mild and reliable reaction process. control, easy post-processing, and avoid side effects

Active Publication Date: 2012-03-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is novel in technology, but the product yield is relatively low. It can be seen from the specific examples that the first step reaction TPP yield of this method is 90%, the second step reaction target product yield is 88~90.6%, and the total yield should be 79.20~ 81.54%, and the second step of the method has harsh reaction conditions, requires high temperature and high vacuum, requires high equipment and relatively high energy consumption, and is difficult to industrialize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add phosphorus oxychloride 11781g, catalyst anhydrous zinc chloride 24.2g and water-absorbing agent phosphorus pentachloride 2.42 in the 20L reaction equipment equipped with stirrer, thermometer, condenser, feeder and hydrogen chloride absorption device g, turn on the condensed water and stirring, heat under stirring until phosphorus oxychloride reflux and keep it for 0.5h; then, cool down to 80-85°C and keep it, and continuously add 2420g of molten resorcinol liquid for 4h, then raise the temperature Continue to react for 1 hour at 110-115°C, and the gas discharged from the reaction is absorbed by the hydrogen chloride absorption device; then, excess phosphorus oxychloride is removed under normal and reduced pressure at 116-140°C to obtain a colorless intermediate product.

[0022] (2) Next, add 48.4 g of catalyst anhydrous zinc chloride and 2.42 g of water-absorbing agent phosphorus pentachloride to the intermediate product from the removal of phosphorus oxychlorid...

Embodiment 2

[0024] (1) In the 20L reaction equipment equipped with stirrer, thermometer, condenser, feeder and hydrogen chloride absorption device, add phosphorus oxychloride 13464g, catalyst anhydrous zinc chloride 36.3g and water-absorbing agent phosphorus pentachloride 7.26 g, turn on the condensed water and stirring, heat under stirring until phosphorus oxychloride reflux and keep it for 0.5h; then, cool down to 80-85°C and keep it, and continuously add 2420g of molten resorcinol liquid for 4h, then raise the temperature Continue to react for 1 hour at 110-115°C, and the gas discharged from the reaction is absorbed by the hydrogen chloride absorption device; then, excess phosphorus oxychloride is removed under normal and reduced pressure at 116-140°C to obtain a colorless intermediate product.

[0025] (2) Next, add 72.6g of catalyst anhydrous zinc chloride and 7.26g of water-absorbing agent phosphorus pentachloride to the intermediate product of phosphorus oxychloride removal, stir an...

Embodiment 3

[0027](1) In the 20L reaction equipment equipped with stirrer, thermometer, condenser, feeder and hydrogen chloride absorption device, add phosphorus oxychloride 15147g, catalyst anhydrous zinc chloride 48.4g and water-absorbing agent phosphorus pentachloride 12.1 g, turn on the condensed water and stirring, heat under stirring until the phosphorus oxychloride refluxes and keep it for 0.5h; then, cool down to 80-85°C and keep it, and continuously add 2420g of molten resorcinol liquid for 4h, then raise the temperature Continue to react for 1 hour at 110-115°C, and the gas discharged from the reaction is absorbed by the hydrogen chloride absorption device; then, excess phosphorus oxychloride is removed under normal and reduced pressure at 116-140°C to obtain a colorless intermediate product.

[0028] (2) Next, add 96.8 g of catalyst anhydrous zinc chloride and 12.1 g of water-absorbing agent phosphorus pentachloride to the intermediate product from the removal of phosphorus oxyc...

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Abstract

The invention relates to a method for preparing retardant resorcin phosphate. The method comprises the following steps: heating phosphorus oxychloride, catalyst and water absorbent until the phosphorus oxychloride flows back; cooling the mixed solvent to a temperature between 80 and 85 DEG C, and adding melted resorcin liquid to the mixed solvent; heating the mixed solvent to a temperature between 110 and 115 DEG C to react so as to obtain an intermediate product, wherein dosage of the catalyst is 1 to 2 percent of the resorcin by weight, dosage of the water absorbent is 0.1 to 0.5 percent ofthe resorcin by weight, and the molar ratio of the phosphorus oxychloride to the resorcin is 3.5-4.5:1; adding the catalyst and the water absorbent into the intermediate product, heating the mixture to a temperature between 120 and 125 DEG C; adding melted phenol liquid to the mixture to obtain a product, wherein dosage of the catalyst is 2 to 4 percent of the resorcin, dosage of the water absorbent is 0.1 to 0.5 percent of the resorcin by weight, and molar ratio of the phenol and the resorcin is 3.75-3.80:1. The content of the resorcin phosphate is more than or equal to 99 percent, content of triphenyl phosphate is less than or equal to 1 percent, so the retardant resorcin phosphate has excellent thermal stability, volatility, migration and durability.

Description

technical field [0001] The invention relates to a preparation method of a halogen-free phosphate flame retardant, in particular to a preparation method of the flame retardant resorcinol phosphate. Background technique [0002] Resorcinol phosphate is a new type of halogen-free phosphate flame retardant, mainly composed of resorcinol bis(diphenyl phosphate) (hereinafter referred to as RDP) and its oligomers, with good flame retardancy, Low vapor pressure, low volatility, low mobility, good thermal stability, low toxicity and environmental protection, etc., so it is widely used in PU (polyurethane), PC (polycarbonate), ABS (acrylonitrile-butadiene-benzene Ethylene copolymer), PC / ABS alloy, PET (polyethylene terephthalate), PP (polypropylene) and other materials are more and more people's attention. [0003] According to literature reports, there are mainly two kinds of synthetic methods about resorcinol phosphate at present, method one: phosphorus oxychloride is reacted with ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/12C09K21/12
Inventor 姜丹蕾刘乃青宋健吕日红韩铁良吴永祥曲世宏吴辉王艳赵英翠
Owner PETROCHINA CO LTD
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