Purification method for tertiary butyl hydroquinone

A technology of tert-butyl hydroquinone and di-tert-butyl hydroquinone, which is applied in the field of purification of tert-butyl hydroquinone, can solve problems such as low process efficiency, and achieve the effect of reducing process cost

Inactive Publication Date: 2012-12-26
XIAMEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Patent JP6228031 uses dioxane and TBHQ and DTBHQ to form complexes in xylene solvent, heats to 80°C and then gradually cools down, TBHQ complexes and DTBHQ complexes are separated out in turn, and then the product is obtained by distilling off the solvent and drying. It is also necessary to solve the residual problem of highly toxic organic solvents during product purification, and the process efficiency is also low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Weigh HQ (0.163g), TBHQ (0.681g) and DTBHQ (0.156g) into a 25ml round bottom flask, then add 5ml of distilled water into the flask and stir at 20°C for 30min, the resulting mixture is used Buchner funnel suction filtration to obtain filter cake. The filter cake was transferred to a 25ml round bottom flask, then 5ml of formic acid was added to the flask and stirred at 20°C for 30min, and the resulting mixture was suction filtered using a Buchner funnel. The filtrate obtained by suction filtration was distilled off under reduced pressure to remove formic acid, and after drying, 0.653 g of white solid powder was obtained. The mass content of TBHQ was 99.07%, the content of DTBHQ was 0.01%, and HQ was not detected by gas chromatography analysis. The recovery rate of TBHQ was 95.0%.

Embodiment 2

[0021] Example 2: Weigh HQ (0.163g), TBHQ (0.681g) and DTBHQ (0.156g) into a 25ml round bottom flask, then add 5ml of distilled water to the flask and stir at 0°C for 30min, the resulting mixture is mixed with a cloth filter through a funnel to obtain a filter cake. The filter cake was transferred to a 25ml round bottom flask, then 5ml of formic acid was added to the flask and stirred at 0°C for 30min, and the resulting mixture was suction filtered using a Buchner funnel. The filtrate obtained by suction filtration was distilled off under reduced pressure to remove formic acid, and after drying, 0.625 g of white solid powder was obtained. The mass content of TBHQ was 99.32%, the content of DTBHQ was 0.01%, and HQ was not detected by gas chromatography analysis. The recovery rate of TBHQ was 91.2%.

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PUM

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Abstract

The invention discloses a purification method for tertiary butyl hydroquinonel, relates to the tertiary butyl hydroquinone, and provides the purification method for the tertiary butyl hydroquinonel, which has the advantages of high efficiency, simple method and capability of meeting national food safety standard. The purification method comprises the following steps of: (1) uniformly mixing hydroquinone, tertiary butyl hydroquinonel and 2,5-ditertbutylhydroquinone, adding water, stirring and then filtering mixture; (2) adding filter cakes obtained by the step (1) into formic acid, recrystallizing, separating out the 2,5-ditertbutylhydroquinone and filtering off the 2,5-ditertbutylhydroquinone; and (3) desolventizing filtrate obtained by the step (2), removing the formic acid to obtain the tertiary butyl hydroquinonel and recycling the formic acid. The content of the obtained tertiary butyl hydroquinonel can reach up to 99 percent.

Description

technical field [0001] The invention relates to tert-butyl hydroquinone, in particular to a method for purifying tert-butyl hydroquinone used in products containing impurities of hydroquinone and 2,5-di-tert-butyl hydroquinone. Background technique [0002] Tert-butyl hydroquinone has many advantages such as no peculiar smell and odor when added to any oil, good safety, high anti-oxidation performance, excellent oil solubility, etc. At the same time, it can effectively inhibit the growth of bacteria and molds, and is effective against Aspergillus flavus It also has a good inhibitory effect on molds that are harmful to human health. It is one of the most excellent phenolic antioxidants at present. It is more effective for unsaturated oils than other commonly used antioxidants such as BHA, BHT, and PG. [0003] According to the national food safety standard (GB26403-2011), food grade tert-butyl hydroquinone requires tert-butyl hydroquinone content ≥ 99.0w%, 2,5-di-tert-butyl h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/08C07C37/70
Inventor 吐松张琛方百发
Owner XIAMEN UNIV
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