Purifying method of antioxidant 168

A purification method and antioxidant technology, applied in the field of antioxidant purification, can solve problems such as difficult to effectively remove impurities, and achieve the effect of being suitable for large-scale production, high yield, and high refining efficiency

Active Publication Date: 2012-10-10
营口风光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently used purification methods include recrystallization methods, usually using solvents such as lower alkanes and ethanol for recrystallization, but the existing recrystallization methods are difficult to effectively remove impurities. With the improvement of quality standards, 2,4-di-tert-butyl The content of phenol is getting higher and higher, so it is necessary to find a way to reduce the content of the impurity 2,4-di-tert-butylphenol in the antioxidant 168, and at the same time prepare an antioxidant with good fluidity and high stability. Agent 168 is an urgent need in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve the crude antioxidant 168 in a mixed solvent (v / v) of ethyl acetate and methanol = 5:1 (w / v) 10 times its weight, heat to reflux temperature for 20 minutes, and let it cool at room temperature. Crystals were precipitated, and crystals were obtained after suction filtration. The above steps were repeated to obtain the second recrystallization product. After drying, the pure product of antioxidant 168 was obtained, with a yield of 96.2%. After HPLC detection, the obtained antioxidant 168 was pure, with a purity of 99.65%. The contents of impurity 1: 2,4-di-tert-butylphenol and impurity 2: 2,4-di-tert-butylphenoxyphosphorus dichloride were all equal. Less than 0.1%.

Embodiment 2

[0026] The detection of product: the product that embodiment 1 method obtains carries out detection result as follows:

[0027] 1. Melting point: 186°C

[0028] 2. Determination of impurity content:

[0029] Methods The HPLC method was adopted, and the chromatographic column was: C18 ODS column (250mm×4.6mm, 5μm); the mobile phase was acetone-methanol (50:50), and the flow rate was 0.5ml·min -1 , the detection wavelength is 275nm, the column temperature is 30 degrees, and the injection volume is 10 microliters. Test results: the content of 2,4-di-tert-butylphenol is 0.0923%; the content of 2,4-di-tert-butylphenoxyphosphorus dichloride is 0.0911%.

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Abstract

The invention relates to a purifying method of an antioxidant 168. The method comprises the following steps that coarse products of the antioxidant 168 are recrystallized for once to three times by mixed solvents consisting of ethyl acetate and carbinol according to a mixture ratio being 5:1, and antioxidant 168 crystals with the purity higher than 99.5 percent are obtained.

Description

technical field [0001] The present invention relates to a method for purifying antioxidants, in particular to a method for purifying antioxidant 168. Background technique [0002] Antioxidant 168, chemical name: tris[2.4-di-tert-butylphenyl] phosphite CAS No. 31570-04-4 Melting range: 183~186℃, density: 1.03g / cm3, bulk density: 0.48~ 0.57g / cm3 [0003] Antioxidant 168 is a phosphite antioxidant with excellent performance developed by Ciba-Geigy in Switzerland. It is an indispensable heat stabilizer in resin processing, which can effectively prevent the generation of hydrogen halide during processing, thereby greatly reducing It can prevent the corrosion of the mold and play a good synergistic effect by decomposing the hydroperoxide formed in the degradation of the polymer. Its characteristics are: strong anti-extraction, stable to hydrolysis, and can significantly improve the light stability of products. It can be widely used in the processing of PP, HDPF, LLDPF, LDPF, ABS...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/145
Inventor 王磊
Owner 营口风光新材料股份有限公司
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