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Preparation methods of substituted diaryl phenol, organophosphorus ester and organic phosphate

A technology of organic phosphate and aryl phenol, which is applied in the field of organic phosphate preparation, can solve problems such as pollution and unfavorable environmental protection, and achieve the effects of overcoming pollution, benefiting environmental protection, and reducing costs

Inactive Publication Date: 2012-12-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the pollution caused by the use of formaldehyde in the prior art, which is unfavorable for environmental protection, and provide a method for preparing substituted diarylphenols and organic phosphates with less pollution and environmental protection. Preparation method and preparation method of organic phosphate

Method used

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  • Preparation methods of substituted diaryl phenol, organophosphorus ester and organic phosphate
  • Preparation methods of substituted diaryl phenol, organophosphorus ester and organic phosphate
  • Preparation methods of substituted diaryl phenol, organophosphorus ester and organic phosphate

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preparation example Construction

[0013] According to the preparation method of substituted diarylphenol of the present invention, in the step (1), the amount of methylal added is, in molar ratio, substituted arylphenol:methylal=1:1-10; Preferably, substituted arylphenol:methylal=1:7-10; more preferably, substituted arylphenol:methylal=1:8-9.

[0014] According to the preparation method of substituted diarylphenols of the present invention, the bridging reaction conditions include: the temperature is 5°C-145°C, and the time is 1-36 hours; preferably, the temperature is 35-80°C, and the time is 3-12 hours. hours; more preferably, the temperature is 60-62° C., and the time is 5-6 hours.

[0015] The catalyst is one or more selected from sulfuric acid, p-toluenesulfonic acid, benzenesulfonic acid, phosphoric acid, and nitric acid; preferably, sulfuric acid, p-toluenesulfonic acid, and benzenesulfonic acid with a concentration of more than 95% by weight one or more of acids; more preferably, one or more of sulfur...

Embodiment 1

[0041] Preparation of substituted diarylphenols Add 41.27 grams of 2,4-di-tert-butylphenol and 150 ml of methylal into the reaction flask, stir until the solid is fully dissolved, slowly add 5 ml of 98% sulfuric acid at room temperature, and dropwise complete Then react at 62°C for 6 hours; then cool down to room temperature, add anhydrous calcium chloride to dehumidify the moisture in the reaction system, then filter, distill to obtain a solid product, and then wash with a large amount of water to adjust the pH to neutral, the obtained Solid product, liquid phase removed. After drying at 80°C, 42.4 g of white solid 2,2'-methylene-bis(4,6-di-tert-butylphenol) was obtained, and the yield based on the amount of 2,4-di-tert-butylphenol was 99.8%, melting point>158°C.

[0042] Preparation of organophosphate: add 42.4 g of the obtained white solid 2,2'-methylene-bis(4,6-di-tert-butylphenol) into the reaction flask, then add 160 ml of toluene and 60 ml of triethylamine, stir When ...

Embodiment 2

[0047] Preparation of substituted diarylphenol: Add 41.35 grams of 4-methyl-6-tert-butylphenol and 160ml of methylal into the reaction kettle, stir until the solid is fully dissolved, and slowly add p-toluenesulfonate at room temperature 3 grams of acid, after the dropwise addition, react at 60°C for 5 hours; then cool down to room temperature, add anhydrous calcium chloride to dehumidify the moisture in the reaction system, wash with a large amount of water to adjust the pH to neutral, and then filter , Distill to obtain a solid product, and then wash the obtained solid product with water to remove the liquid phase. After drying at 80°C, 42.6 g of white solid 2,2'-methylene-bis(4-methyl-6-tert-butylphenol) was obtained, based on the amount of 4-methyl-6-tert-butylphenol The yield was 99.5%, and the melting point was >140°C.

[0048] Preparation of organic phosphate: the white solid 2,2'-methylene-bis(4,6-di-tert-butylphenol) 42.6 is added in the reaction flask, then 160ml of...

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Abstract

The invention relates to a preparation method of substituted diaryl phenol, a preparation method of preparing organophosphorus ester, and a preparation method of organic phosphate. The preparation method of the substituted diaryl phenol comprises the step: under the condition of a bridging reaction, enabling at least one of substituted diaryl phenol shown in a formula (I) to be contacted with methylal and a catalyst to obtain substituted diaryl phenol shown in a formula (II), wherein in the formula (I), R1 is identical to or different from R2; R1 and R2 respectively represent hydrogen atoms or substituted or unsubstituted straight-chain or branched-chain alkyls of C1 to C6; and in the formula (II), R3, R4, R5 and R6 are identical or different and respectively represent substituted or unsubstituted straight-chain or branched-chain alkyls of C1 to C6. According to the preparation method for a nucleating agent, formaldehyde as a bridging agent in the bridging reaction is avoided, and thus the cost can be reduced and the environment friendliness is facilitated.

Description

technical field [0001] The invention relates to a preparation method of a substituted diaryl phenol, a preparation method of an organic phosphate and a preparation method of an organic phosphate. Background technique [0002] Substituted aryl organophosphate metal salts are widely used as nucleating modifiers for polypropylene resins, and are used in the modification of polypropylene resins, where substituted diaryl organophosphate metal salts such as bis(2,4-di-tert-butylphenoxy Base) sodium phosphate, 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)sodium phosphate, etc., can significantly improve the processing properties of these resins (see "High performance of polypropylene - Nucleating agent", "Chemical Industry", 1999(8), p11); "The effect of nucleating agent on the properties of polypropylene", "Synthetic Resins and Plastics", 2001, 18(4), 39-41). [0003] At present, the synthesis of substituted diaryl organophosphate metal salts is to obtain substituted diaryl bisphe...

Claims

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Application Information

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IPC IPC(8): C07C37/16C07C39/16C07F9/12C08L23/12C08K5/523
Inventor 顾民徐耀辉吕静兰李伟褚海斌
Owner CHINA PETROLEUM & CHEM CORP
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