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Method for preparing retardant resorcinol bis(2,6-dimethyl ployphosphate ester)

A technology of dimethyl aryl phosphate and resorcinol, which is applied in the field of preparation of sterically hindered aryl bisphosphate, and achieves the effects of less by-products, reduced energy consumption, and stable process

Active Publication Date: 2010-06-09
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no research report in China. The development of this process and product can break the phenomenon of foreign monopoly, increase the variety of flame retardants, and improve the level of domestic flame retardants.

Method used

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  • Method for preparing retardant resorcinol bis(2,6-dimethyl ployphosphate ester)
  • Method for preparing retardant resorcinol bis(2,6-dimethyl ployphosphate ester)
  • Method for preparing retardant resorcinol bis(2,6-dimethyl ployphosphate ester)

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 93.6 g (0.612 mol) of phosphorus oxychloride, 2.8 g of anhydrous zinc chloride, and 0.1 g of phosphorus pentachloride into a four-neck flask equipped with a stirrer, a thermometer, a condenser, an insulating dropping funnel, and a hydrogen chloride absorption device. g, xylene 18.6g, start the agitator, turn on the cooling water of the condenser, and heat to the temperature of the kettle to be 110~117°C, continuously drop 146.4g (1.2mol) of 2,6-xylenol, in 1~ After the dropwise addition is completed within 2 hours, raise the temperature to 145-150°C and react for 3-4 hours to obtain a colorless intermediate product, and the hydrogen chloride produced is recovered by a hydrochloric acid absorption device;

[0027] Next, the temperature of the intermediate was lowered to about 140°C, and 2.8 g of catalyst anhydrous aluminum chloride was added to the intermediate product, stirred evenly, and 32.4 g of resorcinol was continuously added dropwise for 1 hour. Raise it to a...

Embodiment 2

[0029] Add 93.0 g of phosphorus oxychloride, 2.8 g of anhydrous zinc chloride, 0.1 g of phosphorus pentachloride, and xylene 30g, start the agitator, turn on the cooling water of the condenser, and heat the kettle to a temperature of 110-117°C, add 146.4g (1.2mol) of 2,6-dimethylphenol dropwise continuously, dropwise within 1-2 hours After the end, raise the temperature to 145-150°C and react for 3-4 hours to obtain a colorless intermediate product, and the produced hydrogen chloride is recovered through a hydrochloric acid absorption device;

[0030]Next, the temperature of the intermediate was lowered to about 140°C, 2.0 g of catalyst anhydrous aluminum chloride was added to the intermediate product, stirred evenly, and 32.0 g of resorcinol was continuously added dropwise for 3 hours. Raise it to about 150° C., react for 4 hours, monitor the content of the crude product by liquid chromatography, the 2,6-dimethylphenol content in the crude product is 0.04%, and stop the react...

Embodiment 3

[0032] Add 93g of phosphorus oxychloride, 0.3g of anhydrous zinc chloride, 0.05g of phosphorus pentachloride, and 30g of xylene into a four-necked flask equipped with a stirrer, a thermometer, a condenser, an insulating dropping funnel, and a hydrogen chloride absorption device. , start the agitator, turn on the cooling water of the condenser, and heat the kettle until the temperature is 110-117°C, add 146g of 2,6-dimethylphenol continuously dropwise, after the dropwise addition is completed within 1-2 hours, raise the temperature Reaction at 145-150°C for 3-4 hours to obtain a colorless intermediate product, and the hydrogen chloride produced is recovered through a hydrochloric acid absorption device;

[0033] Next, the temperature of the intermediate was lowered to about 140°C, and 2.5 g of catalyst anhydrous aluminum chloride was added to the intermediate product, stirred evenly, and 32 g of resorcinol was continuously added dropwise for 2 hours. After the dropwise addition,...

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Abstract

The invention relates to a method for preparing resorcinol bis(2,6-dimethyl ployphosphate ester). The method comprises the following steps: heating phosphorus oxychloride, catalyst, water absorbent and solvent to a temperature between 110 and 115 DEG C; dripping 2,6-xylenol into the mixture, wherein the molar ratio of the 2,6-xylenol to the phosphorus oxychloride is 2:(1-1.02) to react at a temperature between 145 and 150 DEG C to obtain a colorless intermediate product; continuously dripping resorcinol into the intermediate product at a temperature between 140 and 145 DEG C, wherein the dosage is 0.48 to 0.5 time that of the molar dosage of the phosphorus oxychloride; reacting at a temperature between 150 and 155 DEG C; cooling the reactant to 100 DEG C to obtain a crude product; and carrying out acid-washing, alkaline-washing, water-washing, evaporating and drying for the crude product to obtain the product. The obtained product has a content of the monomer over 99.0 percent by weight, a melting point between 94.5 and 96.5 DEG C, an acid value less than 0.3mg KOH / g, and good quality.

Description

technical field [0001] The invention relates to a preparation method of sterically hindered aryl bisphosphate, in particular to a preparation method of resorcinol bis(2,6-dimethylaryl phosphate). Background technique [0002] Flame retardants are additives added to plastic products to prevent or inhibit combustion. Common inorganic flame retardants such as magnesium hydroxide, aluminum hydroxide, and polyphosphate amines are added in large amounts, resulting in a decrease in the mechanical properties of the resin. Common organic flame retardants include halogen-based, phosphorus-based and nitrogen-based. Halogen-based flame retardants release hydrogen halide when burned and heated, which is highly corrosive, suffocating and toxic, and may produce dioxins. With the improvement of health and environmental protection requirements, more and more halogen-based flame retardants will fade out of the market; nitrogen-based flame retardants have high hygroscopicity and are easy to pr...

Claims

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Application Information

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IPC IPC(8): C07F9/40C09K21/12
Inventor 姜丹蕾宋健韩铁良吕日红吴永祥曲世宏王芳周亚婷于鸿涛
Owner PETROCHINA CO LTD
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