Preparation method of food additive 3,4-dihydroxy-benzoil acid

A technology of hydroxybenzoate and dihydroxybenzoic acid, applied in the field of food additives, can solve problems such as unfavorable industrialized production, complicated operation, non-compliance with the quality requirements of food additives, etc., and achieve the effect of feasible process conditions and easy availability of raw materials

Inactive Publication Date: 2012-07-25
UNIBEST BIOPHARMA SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Document (Saito, Shizuka; Helvetica Chimica Acta 2006, V89 (7), P1395-1407) has reported the preparation of 3,4-sodium dihydroxybenzoate, according to this document, can only obtain the product that appearance is pink, does not meet as The quality requirements of food additives, and the operation is complicated, which is not conducive to industrial production

Method used

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  • Preparation method of food additive 3,4-dihydroxy-benzoil acid
  • Preparation method of food additive 3,4-dihydroxy-benzoil acid
  • Preparation method of food additive 3,4-dihydroxy-benzoil acid

Examples

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Embodiment 1

[0020] Pretreat the commercially available 3,4-dihydroxybenzoic acid uniformly, take 154g (1 mole), dissolve it in 10-15 times deionized water, add 53-212g (0.5- 2.0 mole) of sodium carbonate, add in about 30 minutes, stir for 2-8 hours, concentrate under reduced pressure until viscous, add 250-800ml of acetone or ethanol, heat up to reflux, then cool to crystallize, filter, and dry to obtain white crystals , yield 95%.

[0021] The present invention can also be realized through the following steps:

[0022] Dissolve 1 mole of pretreated 3,4-dihydroxybenzoic acid in 10-15 times of deionized water, add 0.5-2.0 mole of potassium carbonate at 0-60°C under stirring, and stir for 2-8 hours after adding , concentrated under reduced pressure to the utmost, add 50-400ml of acetone or ethanol, heat up to reflux, then cool to crystallize, filter, and dry to obtain the product.

[0023] Reaction two:

[0024]

Embodiment 2

[0026] Pretreat the commercially available 3,4-dihydroxybenzoic acid uniformly, take 154g (1 mole), dissolve it in 10-15 times deionized water, add 69-276g (0.5- 2.0 mole) of potassium carbonate, add in about 30 minutes, stir for 2-8 hours, concentrate under reduced pressure to a viscous state, add 250-800ml of acetone or ethanol, heat up to reflux, cool to crystallize, filter, and dry to obtain white crystals , yield 95%.

[0027] In the preparation process of the present invention, the consumption of sodium carbonate or potassium carbonate is the key. If the usage is insufficient, the salt formation of 3,4-dihydroxybenzoic acid will be insufficient, and the raw materials will be entrained in the product. If used in excess, the product will have It is pink and does not meet the requirements for food additives.

[0028] The raw materials of the present invention can be bought in the market.

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Abstract

The invention relates to a method for preparing a food additive 3,4-dihydroxybenzoate. The method is realized by the following steps: 1 mole of pretreated 3,4-dihydroxybenzoic acid is dissolved in 10-15 times of deionized water; added with 0.5-2.0 mole of sodium carbonate or potassium carbonate at 0-60 DEG C while stirring; then the mixture is stirred for 2-8 hours after the addition, and is condensed totally under decompression, and is added with 50-400ml of acetone or ethanol; then the mixture is heated to reflux, cooled for crystallization, filtered and dried to obtain the food additive 3,4-dihydroxybenzoate. The method has the beneficial effects that: the raw materials are available, the process conditions are practicable, white crystal meeting the requirements of the food additive can be obtained, thus providing possibility for large-scale industrialized production.

Description

technical field [0001] The invention relates to the field of food additives, in particular to a preparation method of food additive 3,4-dihydroxybenzoate. Background technique [0002] 3,4-dihydroxybenzoic acid (3,4-dihydroxybenzoic acid) is obtained by high-temperature alkali fusion reaction of vanillin, which can be made into photosensitive materials and also used as intermediates of medicines. It can be made into sodium salt or potassium salt, and combined with vitamin sodium, it can be used as a food additive, which has a tendency to replace the traditional food additive sodium benzoate. If it can be widely used in the food industry, its global consumption will be an astronomical figure. Make great efforts to research and promote. [0003] The structural formula is as follows: [0004] [0005] (where: M=Na, K) [0006] Document (Saito, Shizuka; Helvetica Chimica Acta 2006, V89 (7), P1395-1407) has reported the preparation of 3,4-sodium dihydroxybenzoate, according...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A23L3/3508
Inventor 薛小平
Owner UNIBEST BIOPHARMA SHANGHAI
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