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A method and equipment for preparing lipoic acid granules

A technology of lipoic acid and granules, applied in separation methods, chemical instruments and methods, organic chemistry, etc., can solve problems such as small particle size of crystallized products, irregular product shape, and uneven particle size distribution

Active Publication Date: 2021-05-04
SUZHOU FUSHILAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are quality problems in domestic medicinal products, such as the small particle size of crystallized products, uneven particle size distribution, and irregular product shapes, which greatly affect the price of lipoic acid and cause the products to lack competitiveness in the international market.

Method used

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  • A method and equipment for preparing lipoic acid granules
  • A method and equipment for preparing lipoic acid granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040](1) Ring: 500 kg of water, 750kg sodium sodium sulfide, 24kg catalyst tetrabutylammonium bromide, 24 kg of catalyst tetrabutylammonium bromine, stirred at 25 ° C, then add 500 kg6,8-dichloronate, and finally add solid sulfur 92kg. The reaction can be carried out, without the need for an external heat source, and the material is naturally warmed to about 80 ° C, without the external heat source, the reaction is completed, and the lower oil phase enters the hydrolyzate.

[0041](2) Hydrolysis: 15000 kg of water (circulating sleeve), 20 kg of catalyst (tetrabutylammonium bromide), ethyl hydrazine, hydrine alkali, and mixed 12h at 70 ° C, stirred at 70 ° C, stirred at 70 ° C Heat filtrate, filtrate into an acidification kettle, acidified: the filtrate was crystallized to about 25 ° C, and the dilute hydrochloric acid was dried to pH = 1-2, filtered, thicker sulfic acid, filtrate passed the adsorption column (recovered sulfic acid) and electricity The dialysis device enters the hydrol...

Embodiment 2

[0046](1) Ring: 500 kg of water, 750 kg of sodium sulfide, 24kg catalyst (tetrabutylammonium bromide), stirred at 25 ° C, and then add 500 kg6,8-dichloronate at 25 ° C, and then directly add Solid sulfur 92kg. The reaction can be carried out, without the need for an external heat source, and the material is naturally warmed to about 80 ° C, without the external heat source, the reaction is completed, and the lower oil phase enters the hydrolyzate.

[0047](2) Hydrolysis: 15000 kg of water (circulating sleeve), 20 kg of catalyst (tetrabutylammonium bromide), hydrolyzate, hydrauline, liquid base, stirred at 70 ° C, stirred at 70 ° C, stir filtered at 70 ° C The filtrate enters an acidification kettle, acidification: The filtrate is acidified to about 25 ° C, and the hydrochloric acid is added to pH = 1-2, filtered, thicker sulflic acid, and the filtrate enters the hydrolyzed kettle.

[0048](3) The above thioacin and the first solvent (18% by weight of isopropanol, 52 wt% butanone and 30 wt...

Embodiment 3

[0052](1) Ring: 500 kg of water, 750 kg of sodium sulfide, 24kg catalyst (tetrabutylammonium bromide), stirred at 25 ° C, and then add 500 kg6,8-dichloronate at 25 ° C, and then directly add Solid sulfur 92kg. The reaction can be carried out, without the need for an external heat source, and the material is naturally warmed to about 80 ° C, without the external heat source, the reaction is completed, and the lower oil phase enters the hydrolyzate.

[0053](2) Hydrolysis: 15000 kg of water (circulating sleeve), 20 kg of catalyst (tetrabutylammonium bromide), hydrazine (tetrabutylammonium bromide), hydrochloride, liquid base 350 kg, stirred at 70 ° C, stirred at 70 ° C Filtration, filtrate into an acidification kettle, acidified: the above filtrate was crystallized to about 25 ° C, and the hydrochloric acid was dripped to pH = 1-2, filtered, crude sulfic acid, and the filtrate entered the hydrolyzed kettle.

[0054](3) The above thioacin and the first solvent (18% by weight of isopropanol, ...

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Abstract

The invention relates to a method and equipment for preparing lipoic acid granules, comprising: preparing crude lipoic acid, then adding the crude lipoic acid and a first solvent into a crystallization kettle, heating and dissolving, quickly cooling down to 35-10°C, and standing After growing the crystal for 5-10 minutes, add the second solvent, aerate and stir through the stirring paddle, and let the crystal grow for 40-50 minutes to obtain. The invention obtains crystals with uniform particle size distribution, regular product shape and large product particle size, and the obtained crystals are lipoic acid particle crystals.

Description

Technical field[0001]The present invention belongs to the field of sulfic acid, and in particular, the present invention relates to a method and apparatus for preparing sulfic acid particles.Background technique[0002]Sulfic acid is an insoluble pale yellow crystal, which is widely distributed in biological tissues such as animals and plants, and is separated from piglets from the US Reed in 1951. Soluble in organic solvents such as benzene, trichloromethane and ethyl acetate, is hard to dissolve in water, soluble in dilute alkases. There is more sulphic acid in the animal liver, one of the important coenzymes in the dehydrogenase series of pyruvate.[0003]Sulfic acid has two forms of oxidation type (LA) and reduction (DHLA), wherein the LA contains sulfur and carbon atoms, and the electron density is very high, and therefore has a strong oxide.[0004]Sulfuric acid has a general antioxidant anti-oxidation resistance, which has been used for diabetes in Germany for decades, and other me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D339/04B01D9/02
CPCB01D9/00B01D2009/0086C07D339/04
Inventor 钱庆丁建飞唐欢邵明谭雪良石晓青
Owner SUZHOU FUSHILAI PHARMA CO LTD