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Efficient synthesis method of antioxidant 168

A synthesis method and antioxidant technology are applied in the field of efficient synthesis of antioxidant 168, which can solve the problems of high product purification requirements, low product purity, and insufficient effect, and achieve high product yield, high purity, good effect

Inactive Publication Date: 2015-02-25
JIANGMEN DENGZHONGTAI ENG PLASTICS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of a single catalyst, the effect is not good enough. Although the yield is also high, the purity of the product is not high, resulting in higher requirements for product purification in the later stage, longer process flow, and higher production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] ①. Add 252.15g 2,4-di-tert-butylphenol, 5.7g 4-dimethylaminopyridine and 8.5g triethylamine into a 500ml three-necked flask, then mix 387g xylene and 55.35g phosphorus trichloride solution was added slowly, the temperature was raised to 50°C, and the reaction was carried out for 5 hours;

[0020] 2. The reaction solution obtained in step 1. was heated up to 160° C., reacted for 1.5 h, and hydrogen chloride and xylene were distilled out under reduced pressure;

[0021] ③. Cool the reaction solution after vacuum distillation in step ② to 90°C, add isopropanol, stir for 1 hour, then cool to room temperature, filter with suction and dry to obtain 255.2g of antioxidant 168, yield 98.6% (using trioxide Phosphorus is used as the basis to calculate the yield), the melting point is 184.5~185.3°C, and the purity is 99.7%.

Embodiment 2

[0023] ①. Add 252.15g of 2,4-di-tert-butylphenol, 8.8g of 4-dimethylaminopyridine and 8.8g of triethylamine into a 500ml three-necked flask, then mix 276g of xylene and 55.35g of phosphorus trichloride solution was added slowly, heated to 60°C, and reacted for 2 hours;

[0024] 2. The reaction solution obtained in step 1. is warmed up to 130° C., reacted for 5 hours, and distilled out hydrogen chloride and xylene under reduced pressure;

[0025] ③. Cool the reaction solution after vacuum distillation in step ② to 90°C, add isopropanol, stir for 1 hour, then cool to room temperature, filter with suction and dry to obtain 254.9g of antioxidant 168, yield 98.5% (by trioxide The yield is calculated based on phosphorus), the melting point is 184.3~185.2°C, and the purity is 99.8%.

Embodiment 3

[0027] ①. Add 252.15g 2,4-di-tert-butylphenol, 8.5g 4-dimethylaminopyridine and 5.7g triethylamine into a 500 ml three-necked flask, then add 332g xylene and 55.35g phosphorus trichloride The mixture was added slowly, heated to 55°C, and reacted for 3.5 hours;

[0028] ②. The reaction solution obtained in step ① was heated up to 145° C., reacted for 3.5 hours, and distilled hydrogen chloride and xylene under reduced pressure;

[0029] ③. Cool the reaction solution after vacuum distillation in step ② to 90° C., add isopropanol, stir for 1 hour, cool to room temperature, filter and dry to obtain 253.4 g of antioxidant 168, yield 97.9% (by trioxide The yield is calculated based on phosphorus), the melting point is 184.1~185.4°C, and the purity is 99.7%.

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Abstract

The invention discloses an efficient synthesis method of antioxidant 168. The synthesis method specifically comprises the following steps: adding 2,4-di-tert-butyl phenol and a catalyst in a container, and then slowly adding a mixed solution of xylene and phosphorous trichloride, heating to 50-60 DEG.C, and reacting for 2-5 hours, wherein the catalyst is a mixture of 4-dimethylamino pyridine and triethylamine; then, heating a reaction solution to 130-160 DEG.C, reacting for 1.5-5 hours, distilling off hydrogen chloride and xylene at reduced pressure, and then cooling to 90 DEG.C, adding isopropanol, stirring for 0.5-1.5 hours, cooling to room temperature, carrying out suction-filtering, and drying to obtain the antioxidant 168. The 4-dimethylamino pyridine and triethylamine are mixed to serve as a catalyst, the use amount of the catalyst is low, the effect is good, the process is simple, the product yield is high and can reach 97% and more (counted by phosphorous trichloride), and the purity is high, the efficient synthesis method has good industrial production prospect. And the method can be used for the synthesis of the antioxidant 168.

Description

technical field [0001] The present invention relates to the synthesis method of antioxidant, particularly relates to a kind of efficient synthesis method of antioxidant 168. Background technique [0002] Antioxidant 168, chemical name: tris[2.4-di-tert-butylphenyl] phosphite, CASNo. 31570-04-4, melting range: 183-186°C, density: 1.03g / cm3. Appearance is white crystalline powder, odorless, non-toxic, low volatility, insoluble in water, slightly soluble in alcohols, soluble in various hydrocarbon solvents. [0003] Antioxidant 168 is a phosphite antioxidant with excellent performance. It is an indispensable heat stabilizer in resin processing. It can effectively prevent the generation of hydrogen halide during processing, thereby greatly reducing the corrosion of molds and It can decompose the hydroperoxide formed in the degradation of the polymer and play a good synergistic effect. It is one of the commonly used phosphite auxiliary antioxidants in the world. It has good hyd...

Claims

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Application Information

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IPC IPC(8): C07F9/145
Inventor 金良文曾建平严燕
Owner JIANGMEN DENGZHONGTAI ENG PLASTICS CO LTD
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