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Method for preparing pentaerythritol bis-phosphite antioxidant

A pentaerythritol bisphosphite and pentaerythritol technology are applied in the field of preparation of pentaerythritol bisphosphite antioxidants, which can solve the problems of complex purification process of intermediate products, unsuitable for industrialized production, increased cost and the like, and achieve good high-temperature antioxidant performance , Good color protection ability, the effect of reducing production cost

Active Publication Date: 2009-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The intermediate product purification process of this method is complicated, the yield is not high, the cost increases, and it is not suitable for industrial production

Method used

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  • Method for preparing pentaerythritol bis-phosphite antioxidant
  • Method for preparing pentaerythritol bis-phosphite antioxidant
  • Method for preparing pentaerythritol bis-phosphite antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Add 1 mol of pentaerythritol, 2.5 mol of hindered phenol, and 1000 mL of toluene solvent into a 5 L four-necked flask, and add 0.5 g of pyridine as a cyclization catalyst. Access to N 2 , start stirring, and heat in a water bath. When the temperature is constant at 50°C, start to add PCl dropwise 3 . After the dropwise addition, slowly heat to 80°C to make the cyclization reaction proceed smoothly. After reacting for 8h, adopt 31 P NMR Analyze and monitor the reaction process until the reaction of pentaerythritol and phosphorus trichloride is complete at the same time, add 1000mL triethylamine as a replacement catalyst, heat to 110°C, and keep for 10 hours. The obtained material was filtered while hot, added 3256mL of isopropanol, heated to 70°C and stirred, filtered, then added with 1321mL of n-hexane, stirred and filtered, and the obtained filter cake was dried at 90°C to obtain 325g of the product with a yield of 51.4%.

Embodiment 2

[0072] Add 1mol of pentaerythritol and 1000mL of toluene solvent into a 5L four-necked flask, and add 0.65g of weakly basic anion resin as a cyclization catalyst. Access to N 2 , start stirring, and heat in a water bath. When the temperature is constant at 50°C, start to add PCl dropwise 3 . After the dropwise addition, slowly heat to 80°C to make the cyclization reaction proceed smoothly. After reacting for 5h, adopt 31 P NMR Analyze and monitor the reaction process until the simultaneous reaction of pentaerythritol and phosphorus trichloride is complete. Then add 2.2mol of 2,6-di-tert-butyl-p-cresol, and at the same time add 800mL of tributylamine as a replacement catalyst, heat to 110°C and keep for 10 hours, filter the obtained material while it is hot, then add toluene and heat to boiling, room temperature After crystallization and filtration, the filter cake was washed by adding n-heptane, and after filtration, the resulting filter cake was dried to obtain 372 g of ...

Embodiment 3

[0074] Add 1 mol of pentaerythritol and 1000 mL of toluene solvent into a 5 L four-necked flask, and add 0.5 g of pyridine as a cyclization catalyst. Access to N 2 , start stirring, and heat in a water bath. When the temperature is constant at 50°C, start to add PCl dropwise 3 . After the dropwise addition, slowly heat to 80°C to make the cyclization reaction proceed smoothly. After reacting for 8h, adopt 31 P NMR Analyze and monitor the reaction process until the simultaneous reaction of pentaerythritol and phosphorus trichloride is complete. Then add 4mol of 2,4-di-tert-butylphenol, and at the same time add triethylamine as a replacement catalyst, heat to 120°C, keep for 10 hours, filter the obtained material while it is hot, add xylene and heat to boiling, crystallize at room temperature, filter, The filter cake was washed by adding n-heptane, and after filtration, the resulting filter cake was dried to obtain 384 g of product, with a yield of 63.8%.

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Abstract

The invention relates to a method for preparing an antioxidant. Pentaerythritol and phosphorus trichloride are taken as raw materials and subjected to cyclization to give dichloropentaerythritol diphosphite, and dichloropentaerythritol diphosphite is then subjected to substitution reaction with hindered phenol to give pentaerythritol diphosphite which is subjected to separation, washing, drying, and crushing to obtain the antioxidant. The method adopts a one-pot process to prepare the antioxidant, controls the mixing ratio of raw materials of the cylization, analyzes and supervises the reaction process through 31P NMR, saves separation and purification of intermediates, and reduces production costs. The obtained antioxidant is high in purity, used in polypropylene, and has good high temperature antioxygen property and color protecting capacity.

Description

Technical field [0001] The invention relates to a polymer processing aid, and in particular to a preparation method of pentaerythritol bisphosphite antioxidant. Background technique [0002] Antioxidants are important additives in the processing and application of polymer resins, and their applications involve almost all polymers and their products. In recent years, the output of polymer products in my country has grown rapidly, which provides good market prospects for the development and application of antioxidants. Since traditional phosphite antioxidants, such as tris-(2,4-di-tert-butyl)benzene phosphite (commercially known as 168 antioxidant), are prone to yellowing under high temperature conditions, their use is limited. In the application of high-temperature processing fields such as spinning processing, improving the high-temperature stability and color protection capabilities of phosphites has always been a hot spot in the research and development of antioxidants. ...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/524C09K15/32
Inventor 贺黎明张丽英何海龙王伟马京生张浩郝玉春
Owner CHINA PETROLEUM & CHEM CORP
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