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Preparation method of substituted diaryl phosphate

A technology of aryl phosphate and diaryl, which is applied in the field of preparation of substituted diaryl phosphate salts, to achieve the effects of favorable equipment utilization, saving synthesis time, and easy and convenient recovery of solvents

Inactive Publication Date: 2006-06-14
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction system still uses toxic media such as toluene and organic amines, which brings environmental problems to the operating environment and waste liquid post-treatment.

Method used

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  • Preparation method of substituted diaryl phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add 15 grams of p-tert-butylphenol (0.1mol), 4 grams of sodium hydroxide, and 100 mL of cyclohexane into a four-necked flask with a stirrer, water separator and condenser, and reflux at 80°C for 2 hours . Cool to normal temperature, add 9.2ml of phosphorus oxychloride slowly dropwise with constant pressure dropping funnel, and finish dropping in about 30 minutes. Then the temperature was raised to 80° C. under a silicone oil bath and heated to reflux and stirred for 3 hours. Then lower the temperature to 75° C. and maintain this temperature, add 30% by mass of sodium hydroxide aqueous solution, adjust the pH to 12, and stir for 4 hours. The system becomes a white extrudate mixed material. The purification operation is to drain the product with Buchner funnel, wash with water and then with cyclohexane. After vacuum drying, a white solid fine powder of di-p-tert-butyl phosphate sodium salt was obtained, which was weighed. The melting point of the product was greater th...

Embodiment 2

[0032] Add 20.6 g (0.1 mol) of 2,4-di-tert-butylphenol, 4 g of sodium hydroxide, and 100 mL of cyclohexane into a four-necked flask with a stirrer, a water separator, and a condenser. Condensate at reflux for 2 hours. Cool to normal temperature, add 9.2ml of phosphorus oxychloride with constant pressure dropping funnel, slowly add dropwise, about more than 25 minutes to finish dropping. Then the temperature was raised and stirred under reflux under 80° C. silicone oil bath for 3 hours. Then, an aqueous solution of 30% by mass of sodium hydroxide was added dropwise at 75° C. to adjust the pH value to about 12, and stirred under reflux for about 4 hours. The purification operation is to drain the product with Buchner funnel, wash with water and then with cyclohexane. After vacuum drying, a white solid fine powder of di-2,4-di-tert-butylphenyl phosphate sodium salt was obtained, which was weighed. The melting point of the product was greater than 300°C, and the yield was 86% ba...

Embodiment 3

[0034] Add 21.2g (0.05mol) of 2,2'-methylene bis(4,6-di-tert-butylphenol) in a four-necked flask with a stirrer, a water separator and a condenser tube, and 2 grams of hydroxide Sodium, 2mL triphenyl phosphite, add 100mL petroleum ether and heat to reflux temperature (about 80°C), reflux for 3 hours; cool to normal temperature, add 4.8ml phosphorus oxychloride with constant pressure dropping funnel, slowly drop, About more than 30 minutes to drop. Maintain the temperature in the reaction bottle, and react for 5 hours; add dropwise an aqueous solution of 30% by mass of sodium hydroxide, adjust the pH value to about 12, and stir for about 3 hours under reflux. The resulting solution was suction filtered to remove the solvent, then washed with water and petroleum ether several times, and dried in vacuo to obtain a white powder, sodium salt of 2,2-methylenebis(4,6-di-tert-butylphenyl)phosphate, with a melting point of Greater than 300°C. Based on phenol, the yield is 82%.

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Abstract

The present invention relates to the field of organic and high-molecular chemistry, and discloses a preparation method of substituted diaryl phosphate. It is characterized by that said invention uses substituted phenol or substituted diaryl bisphenol as raw material, in the presence of inorganic alkali and non-toxic solvent said invention makes three steps of phenol treatment, condensation reaction and direct alkali-adding aqueous solution salt formation be implemented in one reaction container.

Description

technical field [0001] The invention relates to the field of organic and macromolecular chemistry, in particular to a preparation method of a substituted diaryl phosphate ester salt. Background technique [0002] Phosphate aryl ester salt is an excellent nucleating agent for polyolefin resins. It is non-toxic and tasteless. It can significantly improve the crystallinity, transparency, tensile strength, flexural strength and modulus of polypropylene resin, increase the crystallization speed and Engaging in impact strength, especially in improving the heat-resistant temperature of polypropylene has outstanding effects. It is also used for nucleation modification of polyester including PET and PET. [0003] Usually, the method for synthesizing substituted diaryl phosphate ester salt is to react several hours in an organic solvent by substituted phenol (monophenol) or substituted diaryl bisphenol (bisphenol) and excess phosphorus oxychloride, then add water and hydrolyze, Sepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C08F2/38C08K5/521
Inventor 冯开才林永成王立罗世敬王鲜梅许芳
Owner SUN YAT SEN UNIV
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