3,4-dihydroxybenzaldehyde purification and decolorization method

A technology of dihydroxybenzaldehyde and decolorizing agent, which is applied in the field of purification and decolorization of 3,4-dihydroxybenzaldehyde, can solve problems such as yellowish color and unstable quality, and achieve stable product quality, no secondary pollution, and environmental protection. friendly effect

Active Publication Date: 2015-09-23
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The problem to be solved by the present invention is to provide a method for purifying and decolorizing 3,4-dihydroxybenzaldehyde,...

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation of embodiment 1 decolorizing agent

[0019] 1) Magnesium powder 20-40wt%, iodine-potassium iodide 1-5wt%, polyacrylamide 10-15wt%, edetate disodium 30-50wt%, activated carbon 10-25wt%.

[0020] 2) Among them, the magnesium powder is component A, which is packaged separately; the others are component B, which is packaged separately.

Embodiment 2

[0022] Add 35kg of industrial 3,4-dihydroxybenzaldehyde into 200L pure water, stir and heat to 70°C, and add 500g of composite reduction decolorizer after the solid is completely dissolved (the content of each component is: magnesium powder 25wt%, iodine- Potassium iodide 5wt%, polyacrylamide 15wt%, edetate disodium 30wt%, activated carbon 25wt%), insulated and stirred for 4 hours and then filtered while hot, the filtrate was stirred and cooled to 5°C to crystallize, filtered, dried, and purified and decolorized 32kg of 3,4-dihydroxybenzaldehyde, the recovery rate was 91.4%. After detection and analysis, the product purity is 99.7wt%, and the chromaticity (platinum-cobalt method) of the aqueous solution (20%wt) is 75.

Embodiment 3

[0024] Add 35kg of industrial 3,4-dihydroxybenzaldehyde into 350L pure water, stir and heat to 65°C, add 2000g of composite reducing decolorizer after the solid is completely dissolved (the content of each component is: magnesium powder 30wt%, iodine- Potassium iodide 2wt%, polyacrylamide 10wt%, edetate disodium 43wt%, activated carbon 15wt%), insulated and stirred for 2 hours and then filtered while hot, the filtrate was stirred and cooled to 0 ° C to crystallize, filtered, and dried to obtain purified decolorized 3,4-dihydroxybenzaldehyde 31kg, recovery rate 88.6%. After detection and analysis, the product purity is 99.9wt%, and the chromaticity (platinum-cobalt method) of the aqueous solution (20%wt) is 60.

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Abstract

The invention discloses a 3,4-dihydroxybenzaldehyde purification and decolorization method, comprising the steps of: taking industrial 3,4-dihydroxybenzaldehyde as a raw material; taking a combined reducing agent as a decolorant, wherein the combined reducing agent is formed by proportionately combining solid chemicals such as magnesium powder, iodine-potassium iodide, polyacrylamide and disodium edetate; performing stirring and filtering to obtain filtrate; and cooling and crystallizing the filtrate, so that purified and decolorized 3,4-dihydroxybenzaldehyde is obtained. According to tests, a measured value of product purity of the 3,4-dihydroxybenzaldehyde obtained by using the method of the invention is greater than 99.5 wt%, and chromaticity of an aqueous solution with 20 wt% of 3,4-dihydroxybenzaldehyde is less than 100 (the platinum-cobalt method). The method of the invention has characteristics of having a good effect of purification and decolorization, being simple in post-processing, being stable and non-toxic and causing no secondary pollution. The method is low in decolorant consumption, low in cost, stable in product quality, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for purifying and decolorizing 3,4-dihydroxybenzaldehyde. Background technique [0002] 3,4-Dihydroxybenzaldehyde, also known as catechin aldehyde, is a chemical reagent widely used in organic synthesis and biochemical research, and is also an important pharmaceutical intermediate, which can be used to synthesize a variety of antibiotics and anti-inflammatory drugs. 3,4 dihydroxybenzaldehyde can be condensed with active hydrogen-containing compounds and ammonia derivatives for the synthesis of cyclic condensed protocatechuic aldehyde anti-inflammatory drugs and anti-shock vasoactive drugs dopamine hydrochloride, epinephrine and normethyl adrenaline [0003] In the prior art, usually only brown 3,4-dihydroxybenzaldehyde products can be obtained in industrial production. Chinese patent CN101676253A discloses a method for synthesizing 3,4-dihydroxybenzaldehyde by air catalytic oxidation. Diphenol and glyoxylic acid are ...

Claims

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Application Information

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IPC IPC(8): C07C47/565C07C45/78
CPCC07C45/78C07C47/565
Inventor 郭建国郑琦顾金凤李德峰
Owner SINOPHARM CHEM REAGENT
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