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A kind of preparation method of phosphite antioxidant

A technology of phosphite and biphenyl bisphosphite, which is applied in the field of preparation of phosphite antioxidants, can solve problems such as severe heat release in the decomplexation process, non-recyclable fuming waste residue, and ecological environment impact, and achieve High selectivity, high product yield and easy operation

Active Publication Date: 2017-02-15
广州合成材料研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The phosphite antioxidant tetrakis (2,4-di-tert-butylphenyl)-4,4'-biphenyl bisphosphite reported in the literature has the disadvantage of using a large amount of fuming The solid catalyst is anhydrous aluminum trichloride, and a large amount of non-recyclable fuming waste residue will be produced during the decomplexation process of the intermediate, which will have a serious impact on the ecological environment
In addition, the heat release during the decomplexation process is relatively severe and difficult to control

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  • A kind of preparation method of phosphite antioxidant

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preparation example Construction

[0017] A preparation method of phosphite antioxidant, comprising the following steps:

[0018] 1) Preparation of organomagnesium compound solution: Add magnesium chips into the reactor, and pass a protective atmosphere into the reactor at 10-90°C, add iodine element until the iodine vapor fills the reactor, and then add dropwise to the reactor The solution of 4,4-dibromobiphenyl is heated to reflux, after the dropwise addition, the organic solvent is added dropwise until the reaction system is clear, reacted under reflux for 2-6h, and cooled;

[0019] 2) At -15-20°C, add the above organomagnesium compound solution dropwise to the solution of bis(2,4-di-tert-butylphenyl)phosphorous oxychloride. Insulate for 1-5 hours, then filter, wash, combine filtrates, and filter to obtain magnesium salt solids and filtrates. Remove the solvent in the filtrates to obtain wet white powders, recrystallize with isopropanol, and dry the powders. .

[0020] In step 1), the molar ratio of 4,4-di...

Embodiment 1

[0031] In a three-neck flask equipped with magnetic stirring, a constant pressure dropping funnel, and a reflux condenser, add 4.8 g of polished magnesium chips under anaerobic and water-free conditions, and blow nitrogen at 50°C for 20 minutes. 1.5 g of iodine was added until the iodine vapor filled the reactor. Add dropwise a tetrahydrofuran solution containing 31.2g of 4,4-dibromobiphenyl (the amount of solvent tetrahydrofuran in the solution is 80ml), and heat to reflux at 70°C. After reflux, the color of iodine disappears, and the reaction solution becomes turbid. After the dropwise addition, 67ml of tetrahydrofuran was added dropwise until the reaction solution was clear, reacted under reflux for 3.5h and then cooled to obtain an organomagnesium compound solution containing tetrahydrofuran;

[0032] Move the organomagnesium compound solution obtained above to a constant pressure funnel, and add it dropwise to a tetrahydrofuran solution of bis(2,4-di-tert-butylphenyl)phos...

Embodiment 2

[0035] In a three-necked flask equipped with magnetic stirring, a constant pressure dropping funnel, and a reflux condenser, 5.6 g of polished magnesium chips were added under anaerobic and water-free conditions, and nitrogen gas was introduced at 50°C for 30 minutes. 1.5 g of iodine was added until the iodine vapor filled the reactor. Add dropwise a tetrahydrofuran solution containing 31.2g of 4,4-dibromobiphenyl (the amount of solvent tetrahydrofuran in the solution is 100ml), and heat to reflux at 70°C. After reflux, the color of iodine disappears, and the reaction solution becomes turbid. After the dropwise addition, add 84ml of tetrahydrofuran until the reaction solution is clear, react under reflux for 4.5 hours and then cool to obtain an organomagnesium compound solution containing tetrahydrofuran; after the reaction, extract the reaction solution and wash the unreacted magnesium chips drying;

[0036] Move the organomagnesium compound solution obtained above to a cons...

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Abstract

The invention discloses a method for preparing a phosphite antioxidant. The method comprises the following steps: 1) preparing an organo-magnesium compound solution, namely adding magnesium chips to a reactor, introducing protective atmosphere into the reactor, adding an iodine substance until the reactor is full of iodine vapor, dropwise adding a 4,4-dibromobiphenyl solution to the reactor, heating and refluxing, dropwise adding an organic solvent to the reaction system to clarify after dropwise adding, reacting for 2-6 hours under a reflux state and cooling; 2) dropwise adding the organo-magnesium compound solution to the bi(2,4-di-tert-butylphenyl) chlorophosphite solution at -15 to 20 DEG C, carrying out heat preservation at -10 to 50 DEG C for 1-5 hours after dropwise adding, filtering, washing, merging filtrate and filtering to obtain magnesium salt solid and filtrate, removing the solvent in the filtrate, so as to obtain wet white powder, then recrystallizing by using isopropanol, and drying the powder. The method is mild in process, simple and convenient to operate, high in catalyst selectivity, high in product yield, green and environment-friendly, and the solvent used in reaction can be recovered.

Description

technical field [0001] The invention relates to a preparation method of a phosphite antioxidant. Background technique [0002] Tetrakis(2,4-di-tert-butylphenyl)-4,4’-biphenyl bisphosphite is a phosphite antioxidant. It has excellent high-temperature aging resistance and hydrolysis resistance, so it can be widely used as an auxiliary antioxidant in various plastic substrates such as polypropylene, polyethylene, ABS resin, and polycarbonate. Domestic literature reports that tetrakis(2,4-di-tert-butylphenyl)-4,4'-biphenylbisphosphite is synthesized using biphenyl, phosphorus trichloride and anhydrous aluminum trichloride as main raw materials , under certain conditions, the complex of intermediate 4,4'-biphenylbisphosphine dichloride was prepared by Friedel-Crafts reaction. By adding a decomplexing agent such as phosphorus oxychloride or pyridine, the intermediate 4,4'-biphenylbisphosphine dichloride can be obtained. Finally, the intermediate was prepared by esterification t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/48C08K5/5393
Inventor 谭卓华王庆杨育农李世昌苑丽红
Owner 广州合成材料研究院有限公司