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Method for synthesizing bis-(2,4-di-tert-butyl phenyl) pentaerythritol diphosphite

A technology of dichloropentaerythritol diphosphite and pentaerythritol diphosphite, which is applied in the field of synthesis of antioxidants, can solve the problems of harsh reaction conditions, difficult removal of phenol, and high cost of raw materials, and achieve easy reaction and low price. Effect

Inactive Publication Date: 2008-08-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction conditions are harsh and the cost of raw materials is high; in the second method, the by-product phenol can be recycled
However, the trace amount of phenol in the product is difficult to remove, and the product is prone to yellowing, which limits its application in the fields of food and medicine; the third method, the specific process route has not been publicly reported

Method used

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  • Method for synthesizing bis-(2,4-di-tert-butyl phenyl) pentaerythritol diphosphite
  • Method for synthesizing bis-(2,4-di-tert-butyl phenyl) pentaerythritol diphosphite
  • Method for synthesizing bis-(2,4-di-tert-butyl phenyl) pentaerythritol diphosphite

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Experimental program
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Effect test

Embodiment 1

[0024] The synthetic method of two (2,4-di-tert-butylphenyl) pentaerythritol diphosphite comprises the following steps:

[0025] (1) Synthesis of dichloropentaerythritol diphosphite;

[0026] In the there-necked flask equipped with stirrer, condenser, thermometer, receiver, add 250ml xylene solvent, 0.2mol pentaerythritol 27.2g and 0.27g catalyst, feed nitrogen, start stirring, stirring speed is 300 rpm, in Add 55g of 0.4mol phosphorus trichloride dropwise within 30 minutes, react at 30°C for 4h, and absorb the generated hydrogen chloride gas with 40g of sodium hydroxide solution; depressurize at a temperature of 90°C and a pressure of -0.001Mpa Unreacted phosphorus trichloride was distilled off, and 0.2 g of unreacted pentaerythritol was removed by filtration to obtain a xylene solution of dichloropentaerythritol diphosphite;

[0027] The mol ratio of phosphorus trichloride and pentaerythritol is 2.0: 1;

[0028] By weight, the consumption of the catalyst is 1% of pentaeryt...

Embodiment 2

[0032] The synthetic method of two (2,4-di-tert-butylphenyl) pentaerythritol diphosphite comprises the following steps:

[0033] 1. Synthesis of dichloropentaerythritol diphosphite;

[0034] In a three-necked flask equipped with a stirrer, a condenser, a thermometer, and a receiver, add 250ml of xylene solvent, 27.2g of 0.2mol pentaerythritol and 0.55g of catalyst methylammonium chloride, feed nitrogen, start stirring, and the stirring speed is 500 RPM, drop 60.5g of 0.44mol phosphorus trichloride within 40 minutes, react at 60°C for 3h, and absorb the hydrogen chloride gas generated with 40g of sodium hydroxide solution; at a temperature of 90°C and a pressure of -0.004 Under the condition of Mpa, unreacted phosphorus trichloride is distilled off under reduced pressure, filters out unreacted pentaerythritol 0.1g, obtains the xylene solution of dichloropentaerythritol diphosphite; The mol ratio of phosphorus trichloride and pentaerythritol is: 2.20: 1; By weight, the consumpt...

Embodiment 3

[0038] The synthetic method of two (2,4-di-tert-butylphenyl) pentaerythritol diphosphite comprises the following steps:

[0039] 1. Synthesis of dichloropentaerythritol diphosphite;

[0040] In a three-necked flask equipped with a stirrer, a condenser, a thermometer, and a receiver, add 230ml of xylene solvent, 27.2g of 0.2mol pentaerythritol and 0.9g of catalyst triethylamine, feed nitrogen, start stirring, and the stirring speed is 700 rpm In 50 minutes, 66g of 0.48mol phosphorus trichloride was added dropwise, reacted at 90°C for 1h, and the generated hydrogen chloride gas was absorbed with 40g of sodium hydroxide solution; under the condition of temperature of 90°C and pressure of -0.006Mpa Under reduced pressure, unreacted phosphorus trichloride was distilled off, and 0.2 g of unreacted pentaerythritol was removed by filtration to obtain a xylene solution of dichloropentaerythritol diphosphite; the molar ratio of phosphorus trichloride to pentaerythritol was 2.4:1 ; By w...

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Abstract

The invention discloses a synthesis method of bis (2, 4-dibutylbenzene) pentaerythritol diphosphite, which comprises 1, synthesizing dichloropentaerythritol diphosphite: using xylene as solvent, adding pentaerythritol and catalyst, feeding nitrogen gas, adding phosphorous trichloride and absorbing generated hydrogen chloride gas via sodium hydroxide solution, and purifying reaction product to obtain the dichloropentaerythritol diphosphite, 2, synthesizing bis (2, 4-dibutylbenzene) pentaerythritol diphosphite: adding 2, 4-bis-tert-butylphenol into the reaction product of step 1, feeding nitrogen gas and mixing, absorbing generated hydrogen chloride gas via sodium hydroxide solution, and purifying the reaction product to obtain final product. The invention uses 2, 4-bis-tert-butylphenol, pentaerythritol and phosphorous trichloride as main materials, with low cost, easily processed reaction and high reaction yield.

Description

technical field [0001] The present invention relates to a synthesis method of an antioxidant, in particular to a new synthesis method of bis(2,4-di-tert-butylphenyl)pentaerythritol diphosphite. Background technique [0002] The structural formula of two (2,4-di-tert-butylphenyl) pentaerythritol diphosphites is: [0003] [0004] Because in this molecule, there are free radical scavenger pentaerythritol group and hydroperoxide decomposing agent phosphite group, the free radical scavenger and hydroperoxide decomposing agent are compounded in one molecule, therefore, this compound It is a molecular compound antioxidant and heat stabilizer. It is used together with hindered phenolic or hindered amine stabilizers, both of which can produce synergistic effects. The trade name is antioxidant 626. It is a new type of high-performance phosphorus-containing antioxidant with excellent prospects. [0005] Bis(2,4-di-tert-butylphenyl)pentaerythritol diphosphite is widely used as aux...

Claims

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Application Information

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IPC IPC(8): C07F9/6571
Inventor 潘朝群
Owner SOUTH CHINA UNIV OF TECH
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