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A method of producing electronic grade gallic acid

A gallic acid and electronic-grade technology, which is applied in the field of producing electronic-grade gallic acid, can solve the problems of many impurities, easy crystallization and blockage, and shorten the service life of resin, and achieve the effect of simplifying the process flow, obvious cost advantages, and extending the service life

Active Publication Date: 2011-12-21
先微康新材料科技有限公司
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AI Technical Summary

Problems solved by technology

Acid hydrolysis and alkali hydrolysis are methods of hydrolyzing gallic acid under the action of sulfuric acid or caustic soda. The basic process is divided into hydrolysis, pressure filtration, crude product crystallization, crude product centrifugation, crude product decolorization, filtration, fine crystal crystallization, fine crystal centrifugation, The finished product is obtained by vacuum drying and pulverization; sulfuric acid in the acid hydrolysis method has strong oxidizing properties, and will destroy a part of the benzene ring structure in the tannic acid during the reaction process, and the color of the crude product is very dark, and there are side reactions, and there are many impurities. It is difficult for the product processed in the subsequent process to meet the standard of electronic-grade gallic acid; the amount of caustic soda and hydrochloric acid used in the alkali hydrolysis method is very high, and the caustic soda and hydrochloric acid are neutralized to form sodium chloride, and the product contains a large amount of sodium chloride after the subsequent process. The processed products also fail to meet the standards of electronic grade gallic acid; the common disadvantages of the acid hydrolysis and alkali hydrolysis processes are: incomplete hydrolysis of tannins, low yield of gallic acid, unstable product quality, serious corrosion of equipment, production The cost is high, and more importantly, the organic wastewater pollutes the environment seriously
The microbial fermentation method uses microorganisms to ferment in an aqueous solution containing tannins, and uses glucose after hydrolysis of tannic acid as a carbon source for the growth and reproduction of microorganisms. At the same time, microorganisms are induced to produce enzymes in the solution, and tannic acid Gallic acid is produced by enzyme-catalyzed hydrolysis; the disadvantages of microbial fermentation are: long production cycle, incomplete hydrolysis, 10-20% tannin unhydrolyzed after fermentation, and product quality not up to the standard of electronic grade gallic acid
Shortcoming in this method: 1, produce a large amount of waste water in the production process (production 1 ton of electronic grade gallic acid produces 16 tons of waste water); 3. The resin is often adsorbed in the environment of 60-75 ℃, which will easily break the resin and shorten the service life of the resin; 4. Although this method can produce electronic grade gallic acid in one step, the cost is high. higher

Method used

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  • A method of producing electronic grade gallic acid
  • A method of producing electronic grade gallic acid
  • A method of producing electronic grade gallic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) The seed cultivation of Aspergillus niger (Aspergillus niger) of No.3.3150 of China General Microorganism Culture Collection and Management Center

[0030] Aspergillus niger seed medium is (unit: W / V): 0.5% tannic acid, 1.2% glucose, 0.1% peptone, 0.05% citric acid, 1% NH 4 CL, 0.3%KH 2 PO 4 , 0.3% Na 2 HPO 4 .12H 2 O, 0.05% MgSO 4 .7H 2 O, agar 3%; cultured at 30°C, 140r / min for 38 hours.

[0031] (2) Aspergillus niger fermentation enzyme production

[0032] Aspergillus niger fermentation enzyme medium is (unit: W / V): 1.0% glucose, 0.5% sucrose, 0.1% peptone, 0.05% citric acid, 0.4% soluble starch, 1% NH 4 CL, 0.3%KH 2 PO 4 , 0.3% Na 2 HPO 4 .12H 2 O, 0.1% KCl, 0.03% CaCl 2 , 0.05% MgSO 4 .7H 2 O, 8% tannic acid; transfer to the fermentation medium of tannic acid with 6% (W / V) inoculation amount, 26~30 ℃, cultivate 70~75 hours under the condition of 130~140r / min, filter to obtain Enzyme solution.

[0033] (3) Enzymatic hydrolysis

[0034] Put 15K...

Embodiment 2

[0044] (1) The seed cultivation of Aspergillus niger (Aspergillus niger) of No.3.3150 of China General Microorganism Culture Collection and Management Center

[0045] Aspergillus niger seed medium is (unit: W / V): 0.5% tannic acid, 1.2% glucose, 0.1% peptone, 0.05% citric acid, 1% NH 4 CL, 0.3%KH 2 PO 4 , 0.3% Na 2 HPO 4 .12H 2 O, 0.05% MgSO 4 .7H 2 O, agar 3%; cultured at 30°C, 140r / min for 38 hours.

[0046] (2) Aspergillus niger fermentation enzyme production

[0047] Aspergillus niger fermentation enzyme medium is (unit: W / V): 1.0% glucose, 0.5% sucrose, 0.1% peptone, 0.05% citric acid, 0.4% soluble starch, 1% NH 4 CL, 0.3%KH 2 PO 4 , 0.3% Na 2 HPO 4 .12H 2 O, 0.1% KCl, 0.03% CaCl 2 , 0.05% MgSO 4 .7H 2 O, 6% tannic acid; transfer to tannic acid fermentation medium with 5% inoculum amount, cultivate for 70-75 hours at 26-30° C., 130-140 r / min, and filter to obtain enzyme liquid.

[0048] (3) Enzymatic hydrolysis

[0049] Put 20Kg of Tara powder with 48% ta...

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Abstract

The invention discloses a method for producing electronic-grade gallic acid by using tara powder as a raw material through microbial fermentation and resin adsorption. Tara powder is used as raw material to produce electronic-grade gallic acid by microbial fermentation combined with resin adsorption, and Tara powder is fermented with Aspergillus niger to produce crude gallic acid. Then, the ethanol was evaporated under reduced pressure to recover the ethanol until the crystals were precipitated, and the refined gallic acid was obtained by cooling and filtration, and the electronic grade gallic acid was obtained after vacuum drying. Na, Fe, K, Ca, Mg, Cu, Zn, Al, Mn ions are all ≤50ppb. The method has the advantages of no pollution, high yield, low cost, recyclable resin and no damage to the resin, and is suitable for washing integrated circuits with detergent in the electronic industry.

Description

technical field [0001] The invention relates to a method for producing electronic-grade gallic acid by using tara powder as a raw material through microbial fermentation and resin adsorption. Background technique [0002] High-purity chemicals for the electronics industry, namely MOS reagents (Moss reagents). Generally used in semiconductors, electron tubes, integrated circuit boards, etc., the highest impurity content is 0.01-10ppm, and some can be reduced to ppb levels. The dust level reaches 0-2ppb. The production of electronic-grade reagents generally uses industrial-grade products as raw materials, and the corresponding purification technology is used to remove impurities in the raw materials according to the characteristics of the raw materials. [0003] Gallic acid is also called double acid and gallic acid, its chemical name is 3,4,5-trihydroxybenzoic acid (3,4,5-trhydroxybenzoic acid), and its molecular formula is (OH 3 )C 6 h 2 COOH.H 2 O, the structural form...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P7/42C07C65/03C07C51/47C07C51/44C12R1/685
Inventor 罗伟
Owner 先微康新材料科技有限公司
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