Preparation method for organic phosphate nucleating agent

A technology of organic phosphate and organic phosphate, applied in organic chemistry, phosphorus organic compounds, chemical instruments and methods, etc., can solve the problems of low nucleating agent yield, high solvent toxicity, poor solubility, etc., and achieve reaction efficiency High, easy solvent recovery, strong solvency effect

Active Publication Date: 2009-02-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that benzene non-polar organic solvents are used in the phosphorylation reaction, the solubility is poor, the yield of the nucleating agent is low, the solvent used is highly toxic, the price is high, and the recovery is difficult

Method used

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  • Preparation method for organic phosphate nucleating agent
  • Preparation method for organic phosphate nucleating agent
  • Preparation method for organic phosphate nucleating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 2,2'-methylene-bis(4,6-di-tert-butylphenol) 42.4g, dichloromethane 160ml and triethylamine 50ml into the reaction flask, stir until the solid is fully dissolved, and slowly Slowly add 20ml of phosphorus oxychloride, and react at room temperature for 12 hours after the dropwise addition; then add 150ml of water and stir for 1.5hr, then evaporate the solvent, filter and wash with water to obtain a solid product, purify the solid product with ethanol, remove the liquid phase, and dry Afterwards, 48.6 g of a white solid was obtained, which was the intermediate product 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)phosphate, and the yield of the intermediate product was 99.8%.

[0053] Then dissolve the intermediate product in a mixture of acetone and water, add aqueous sodium hydroxide solution to form a salt and neutralize it, and distill off the acetone to obtain a white solid product. After filtering, wash with deionized water until the pH value is neutral. After heati...

Embodiment 2

[0055] Add 42.4g of 2,2'-methylene-bis(4,6-di-tert-butylphenol), 150ml of dibromomethane and 45ml of triethylamine into the reaction flask, stir until the solid is fully dissolved, and slowly Add 20ml of phosphorus oxychloride, react at room temperature for 12 hours after the dropwise addition; then add 150ml of water and stir for 1.5hr, then evaporate the solvent, filter and wash with water to obtain a solid product, purify the solid product with ethanol, remove the liquid phase, and dry 48.3 g of white solid was obtained, which was the intermediate product 2,2'-methylene-bis(4,6-di-tert-butylphenoxy)phosphate, and the yield of the intermediate product was 99.4%.

[0056] Then dissolve the intermediate product in a mixture of acetone and water, add aqueous sodium hydroxide solution to form a salt and neutralize it, and distill off the acetone to obtain a white solid product. After filtering, wash with deionized water until the pH value is neutral. After heating and drying, 46...

Embodiment 3

[0058] Add 42.4g of 2,2'-methylene-bis(4-methyl-6-tert-butylphenol), 170ml of chloroform and 52ml of triethylamine into the reaction flask, stir until the solid is fully dissolved, and Slowly add 22ml of phosphorus oxychloride, and react at room temperature for 12 hours after the dropwise addition; then add 150ml of water and stir for 1.5hr, then evaporate the solvent, filter and wash with water to obtain a solid product, purify the solid product with ethanol, and remove the liquid phase , to obtain 49.6g of white solid after drying, which is the intermediate product 2,2'-methylene-bis(4-methyl-6-di-tert-butylphenoxy) phosphate, and the yield of the intermediate product is 99% %.

[0059] Then dissolve the intermediate product in a mixture of acetone and water, add aqueous sodium hydroxide solution to form a salt and neutralize it, and distill off the acetone to obtain a white solid product. After filtering, wash with deionized water until the pH value is neutral. After heati...

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Abstract

The present invention relates to a method for preparing an organic compound, in particular to a method for preparing an organic phosphate nucleator, which includes the following steps: phosphorylation reaction, hydrolyzation and salification. Since the solvent for the phosphorylation reaction adopts halogenated hydrocarbon instead of benzene series compounds, which is cheap, the cost can be reduced, and since the yield of the organic phosphate synthesized with the halogenated hydrocarbon used as the solvent is higher, the yield of the final product, the organic phosphate, is greatly increased. Moreover, since the solvent does not adopt the benzene series compounds, toxicity is low, non-burning operation is safe, environment can be protected, recycling is convenient, and the diaryl-substituted organophosphate metal salt used as nucleator prepared by the method has obvious effect in the improvement of the processing property of resin.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of a substituted diaryl organophosphate metal salt. 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. The above content can be found in the scientific literature "High Performance of Polypropylene-Nucleating Agent" ("Chemical Industry", 1999 (8), p11), "Influence of Nucleating Agent on the Properties of Polypropylene" ("Synthetic Resin and Plastics" , 2001, 18(4), 39-41). [0003] At present, the synthesis of substituted aryl organophosphate metal salt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C07F9/12C08K5/521
Inventor 顾民吕静兰张丽英李伟徐耀辉张浩
Owner CHINA PETROLEUM & CHEM CORP
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