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HMB-Ca production process method

A production process, a technology of hmb-ca, applied in chemical instruments and methods, oxidation preparation of carboxylic acid, carboxylate preparation, etc., can solve problems such as many steps, high risk, and unfavorable industrialization.

Inactive Publication Date: 2018-06-08
穆云
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the parameter conditions of the laboratory small-scale preparation method of HMB-Ca cannot meet the needs of scale-up production. It is necessary to optimize and adjust the condition parameters during the scale-up production of HMB-Ca products, and it is necessary to optimize the subsequent purification of HMB-Ca products in the production process. Operation methods to meet the requirements of HMB-Ca products in terms of mechanical impurities and metal ion quality
Moreover, the small-scale preparation method of HMB-Ca laboratory disclosed in the prior art still has the following disadvantages: (1) the preparation method has many steps, the process is complicated and difficult to operate, the reaction conditions are harsh, and the total yield is low; (2) ) produces a large amount of waste water and waste liquid during the preparation process, which pollutes the environment; (3) uses flammable and explosive reagents, which is dangerous, and the feeding and post-processing operations are cumbersome and costly, which is not conducive to industrialization
In view of the many defects of the above-mentioned existing preparation methods, and in view of the fact that the existing preparation methods cannot meet the quality requirements of the enlarged production of HMB-Ca products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] The production operation of embodiment 1, β-hydroxyl-β-methylbutyric acid

[0082] Step 1. Control the temperature at 10°C, add 80Kg of diacetone alcohol into 1200L of sodium hypochlorite aqueous solution (10%), stir at room temperature for 4 hours, let the layers stand, remove the lower liquid, and wash the upper reaction liquid;

[0083] Step 2. Add 14Kg of sodium bisulfite to the upper reaction solution in step 1, stir at 10°C, add 160L of concentrated hydrochloric acid solution, adjust the pH to 2, concentrate under reduced pressure to remove water, and filter to obtain β-hydroxy-β - methyl butyric acid crude product solution;

[0084] Step 3, add 640 L of ethyl acetate to the crude product solution of β-hydroxy-β-methylbutyric acid obtained in step 2 for extraction, combine the extracted organic phases and add anhydrous sodium sulfate to dry for 4 hours, filter, and concentrate the filtrate at 60°C to obtain 63Kg β-Hydroxy-β-methylbutyric acid compound.

[0085] ...

Embodiment 2

[0086] The production operation of embodiment 2, β-hydroxyl-β-methylbutyric acid

[0087] Step 1, control the temperature at 15°C, add 150Kg of diacetone alcohol into 2700L sodium hypochlorite aqueous solution (15%), stir at room temperature for 5 hours, let stand to separate layers, separate the lower liquid, and wash the upper reaction liquid;

[0088] Step 2. Add 27Kg of sodium bisulfite to the upper reaction solution in step 1, stir at 20°C, add 150L of concentrated hydrochloric acid solution, adjust the pH to 3, concentrate under reduced pressure to remove water, and filter to obtain β-hydroxy-β - methyl butyric acid crude product solution;

[0089] Step 3. Add 1350 L of ethyl acetate to the crude product solution of β-hydroxy-β-methylbutyric acid obtained in step 2 for extraction, combine the extracted organic phases and add anhydrous sodium sulfate to dry for 6 hours, filter, and concentrate the filtrate at 90°C to obtain 114Kg β-Hydroxy-β-methylbutyric acid compound. ...

Embodiment 3

[0091] The production operation of embodiment 3, β-hydroxyl-β-methylbutyric acid

[0092] Step 1, control the temperature at 5°C, add 200Kg of diacetone alcohol into 2000L sodium hypochlorite aqueous solution (20%), stir at room temperature for 3 hours, let stand to separate layers, separate the lower liquid, and wash the upper reaction liquid;

[0093] Step 2. Add 40Kg of sodium bisulfite to the upper reaction solution of step 1, stir at 15°C, add 600L of concentrated hydrochloric acid solution, adjust the pH to 2, concentrate under reduced pressure to remove water, and filter to obtain β-hydroxy-β - methyl butyric acid crude product solution;

[0094] Step 3, add 1000 L of isobutanol to the crude product solution of β-hydroxy-β-methylbutyric acid obtained in step 2 for extraction, combine the extracted organic phases and add anhydrous sodium sulfate to dry for 18 hours, filter, and concentrate the filtrate at 80°C to obtain 162Kg β-Hydroxy-β-methylbutyric acid compound.

...

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PUM

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Abstract

The invention discloses HMB-Ca production process method, which comprises the following steps that HMB is dissolved in water; calcium salt is added; stirring, filtering and concentration are performedto obtain an HMB-Ca crude product; the HMB-Ca crude product is added into an alcohol solvent; after stirring, filtering and concentration are performed, an organic solvent is added; stirring and filtering are performed; solid drying is performed to obtain an HMB-Ca product; during the filtering, the hole diameter is 1 to 100 micrometers. The HMB-Ca production process method has the advantages that the production operation and purification filtering conditions of the HMB-Ca product are optimized; the mechanical impurities and the metal ion residues in the HMB-Ca product are effectively reduced; the safety when the HMB-Ca product is used as a health care product and food additive is improved; the process conditions are mild; the operation is easy; the production operation safety degrade isreduced; green and environment-friendly effects are achieved; the industrialization is favorably realized.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a production process of HMB-Ca. Background technique [0002] The compound β-hydroxy-β-methylbutyrate calcium, referred to as HMB-Ca, is a metabolite of leucine. HMB-Ca can be used to promote animal muscle growth, enhance the immune ability of mammals, reduce cholesterol and low-density lipoprotein (LDL) levels in the human body to reduce the incidence of coronary heart disease and cardiovascular disease, and can also help the human body to supplement calcium and strengthen the human body. Nitrogen fixation ability to maintain protein levels in the body; therefore, it is widely used and can be added to beverages, milk and dairy products, cocoa products, chocolate and chocolate products, as well as candy, baked goods, and special diets as food additives, dietary additives, and weight loss food additives In food, it can supplement calcium, lose weight, build muscle, enha...

Claims

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Application Information

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IPC IPC(8): C07C59/01C07C51/41C07C51/43C07C51/16
CPCC07C51/16C07C51/412C07C51/43C07C59/01
Inventor 不公告发明人
Owner 穆云
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