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Di-2,4-dicumylphenyl pntaerythritol dphosphite preparation method

A technology of cumylphenyl pentaerythritol bisphosphite and pentaerythritol, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve complex operations, poor quality, and product yield. Low-level problems, to achieve good technical effects, product quality and yield improvement

Active Publication Date: 2008-11-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is to overcome the shortcomings of low product yield, poor quality and complicated operation when preparing di-2,4-dicumylphenylpentaerythritol bisphosphite in the previous literature, and provide a new The preparation method of di-2,4-dicumylphenyl pentaerythritol diphosphite

Method used

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  • Di-2,4-dicumylphenyl pntaerythritol dphosphite preparation method

Examples

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Embodiment 1

[0020] A 500ml four-neck flask is equipped with stirring, thermometer, dropping funnel, reflux condenser and hydrogen chloride escape absorption device respectively. Weigh 75 grams of 2,4-dicumylphenol and 0.6 grams of triethylamine, dissolve them in 60 grams of toluene and 60 grams of n-hexane, raise the temperature to 35°C, and add 31.3 grams of phosphorus trichloride dropwise under the protection of nitrogen. After 1 hour, the temperature was raised to reflux after dropping, and kept for 2 hours. A total of 30 grams of unreacted phosphorus trichloride and a small amount of solvent were evaporated under reduced pressure, and 30 grams of fresh toluene / n-hexane mixed solution (toluene weight / n-hexane weight=1) was added. Cool down to 45°C, add 15.4 g of pentaerythritol, stir vigorously for 2 hours, raise the temperature to reflux, and keep the temperature for 4 hours. The solvent was distilled off under reduced pressure, 100 g of absolute ethanol was added to the remaining so...

Embodiment 2

[0022] The configuration of the 500 milliliter four-necked flask is the same as in Example 1, except that 0.6 gram of tri-n-butylamine is used to replace 0.6 gram of triethylamine, and 120 gram of normal hexane is used to replace the mixed solution of 60 gram of toluene and 60 gram of normal hexane, add 30 gram of fresh n-hexane to replace 30 grams of mixed solution of toluene and n-hexane (toluene weight / n-hexane weight=1). After the same post-treatment, 70.6 grams of white powdery fluid solids were obtained, with a yield of 73.2%, a melting point of 229.8° C., a purity of 97.2% as measured by DSC differential scanning method, an acid value mg KOH / g of 0.91, and a P content of 7.46%.

Embodiment 3

[0024] 500 milliliters of four-necked flask configurations are the same as embodiment 1, and difference is to replace the mixed solution of 60 gram toluene and 60 gram normal hexane with 120 gram toluene, add the mixed solution (toluene Weight / weight of n-hexane=1). In the post-treatment, anhydrous methanol was used instead of absolute ethanol for purification to obtain 77.6 grams of white powdery mobile solid with a yield of 80.4% and a melting point of 230.8°C. The purity was 98.3% as measured by DSC differential scanning method, and the acid value was mg KOH / g was 0.87, and the P content was 7.35%.

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Abstract

The invention relates to a method for preparing double- 2, 4- biscumidic phenyl pentaerythrite bis-phosphite ester, and aims to solve problems of low productivity, poor quality and complicate operation. The invention employs organic amine as catalyst, toluene and skellysolve B or mixing solution of them as dissolvent, proceeds reaction with 2, 4- bis-cumidic carbolic acid and phsophorus trichloride, prepares said product with generated compound and pentaerythrite through esterification. The product can be used in industrial preparation of polyethylene, polypropylene and ABS and so on.

Description

technical field [0001] The invention relates to a preparation method of di-2,4-dicumylphenyl pentaerythritol bisphosphite antioxidant. Background technique [0002] As we all know, polymers and their products will inevitably undergo structural changes during preparation, processing and application, which will damage their strength and appearance until they lose their use value. This phenomenon is called the aging of polymer materials. The aging of polymer materials is an irreversible process, which is mainly caused by external factors such as light, oxygen, and heat. Among them, the auto-oxidation reaction caused by oxygen can be carried out at lower temperature and occurs more easily than pure thermal decomposition reaction, so oxidative degradation is more important than pure thermal decomposition. In order to effectively prevent the aging of polymer materials, substances that can inhibit or delay the oxidative degradation of polymers during manufacturing, processing and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/145
Inventor 沈之芹王芳李斌傅荣政
Owner CHINA PETROLEUM & CHEM CORP
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