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Beta-hydroxyl-beta-methyl calcium butyrate preparation method

A technology of calcium methyl butyrate and methyl butyric acid, applied in the field of nutritional fortifiers, can solve the problems of non-conformity with green chemistry, high cost, pollution, etc., and achieves a synthesis method with high efficiency and environmental protection, broad market prospects, and mild reaction. Effect

Inactive Publication Date: 2018-04-24
JINHU SHENKAI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the preparation of β-hydroxy-β-methylbutyrate calcium by the prior art, there are still problems of high cost, low efficiency, and pollution. It does not conform to the concept of green chemistry, and it is difficult to promote production on a large scale

Method used

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  • Beta-hydroxyl-beta-methyl calcium butyrate preparation method

Examples

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Effect test

Embodiment 1

[0041] Mix 200ml of sulfuric acid solution with a mass concentration of 10% with 2000ml of glacial acetic acid and 6000ml of hydrogen peroxide with a mass concentration of 30%, and react at 45°C for 10min, during which the stirring speed is 200rpm. Fraction, obtain 2500ml of peracetic acid aqueous solution, mix it with 1250ml of diacetone alcohol, add 2000ml of methyl acetate, react at 30°C for 1h, during which the stirring speed is 100rpm, distill and collect the fraction at 70°C to obtain methyl acetate, The substance after distillation is β-hydroxy-β-methylbutyric acid solution, add water 2500ml therein, then add sodium hydroxide solution to adjust to pH 6.0, filter after heating to dissolve, take filtrate and add 1000g calcium chloride. Stir and react at 400rpm for 20min, add sodium hydroxide to adjust the pH to 6.5, precipitate β-hydroxyl-β-methylbutyrate calcium, filter, and dry to obtain β-hydroxyl-β-methylbutyrate calcium 1704g. It is put into the feeding system 600, e...

Embodiment 2

[0043]Mix 200ml of 10% sulfuric acid solution with 1800ml of glacial acetic acid and 5400ml of 30% hydrogen peroxide at 50°C for 12 minutes with a stirring speed of 250rpm. Fraction, obtain 1900ml of peracetic acid aqueous solution, mix it with 1100ml of diacetone alcohol, add 2000ml of methyl acetate, react at 35°C for 70min, during which the stirring speed is 120rpm, distill and collect the fraction at 70°C to obtain methyl acetate, The substance after distillation is β-hydroxy-β-methylbutyric acid solution, add water 2100ml to it, then add sodium hydroxide solution to adjust the pH to 6.0, heat to dissolve and filter, take the filtrate and add 1000g calcium chloride. Stir and react at 450rpm for 30min, add sodium hydroxide to adjust the pH to 6.5, precipitate β-hydroxyl-β-methylbutyrate calcium, filter, and dry to obtain β-hydroxyl-β-methylbutyrate calcium 1690g. It is put into the feeding system 600, enters the crushing system 500 for crushing, and then is collected by the...

Embodiment 3

[0045] Mix 200ml of sulfuric acid solution with a mass concentration of 10%, 2000ml of glacial acetic acid, and 5000ml of hydrogen peroxide with a mass concentration of 30%, and react at 40°C for 10min, during which the stirring speed is 200rpm. Fraction, obtain 1800ml of peracetic acid aqueous solution, mix it with 900ml of diacetone alcohol, add 1600ml of methyl acetate, react at 25°C for 50min, the stirring speed is 120rpm, distill and collect the cut at 70°C to obtain methyl acetate, The substance after distillation is β-hydroxy-β-methylbutyric acid solution, add water 2300ml to it, then add sodium hydroxide solution to adjust the pH to 6.0, heat to dissolve and filter, take the filtrate and add 1000g calcium chloride. Stir and react at 350rpm for 30min, add sodium hydroxide to adjust the pH to 6.5, and precipitate β-hydroxyl-β-methylbutyrate calcium, filter, and dry to obtain β-hydroxyl-β-methylbutyrate calcium 1650g. It is put into the feeding system 600, enters the crus...

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Abstract

The invention discloses a beta-hydroxyl-beta methyl calcium butyrate preparation method which comprises the steps: mixing sulfuric acid, glacial acetic acid and hydrogen peroxide, performing primary constant-temperature reaction and distilling and collecting peracetic acid; mixing peracetic acid and diacetone alcohol, adding methyl acetate, performing secondary constant-temperature reaction and distilling and collecting beta-hydroxyl-beta methylbutyric acid; adding water into the beta-hydroxyl-beta methylbutyric acid, adjusting a solution pH, heating, dissolving and filtering, taking filtrateand adding calcium chloride, stirring and reacting, adjusting a pH, separating out beta-hydroxyl-beta-methyl calcium butyrate, filtering and drying to obtain the beta-hydroxyl-beta methyl calcium butyrate and superfinely grinding to obtain a product. The beta-hydroxyl-beta methyl calcium butyrate prepared by the preparation method disclosed by the invention has the advantages of high yield, high-efficiency and environment-friendly in synthesizing method, ability in meeting a green chemical synthesizing idea and a wide market prospect.

Description

technical field [0001] The invention belongs to the technical field of nutrition enhancers, and in particular relates to a preparation method of calcium beta-hydroxy-beta-methylbutyrate. Background technique [0002] β-Hydroxy-β-methylbutyrate (β-Hydroxy-β-Methyl Butyrate, HMB, molecular formula C 5 h 10 o 3 ) is an intermediate metabolite of the essential amino acid leucine. Leucine is a branched-chain amino acid, which is an essential amino acid. It cannot be produced in the body and is very important to human health. Humans must rely on diet to ensure the intake of leucine. HMB is an intermediate metabolite of leucine. Food contains HMB, and the human body can produce a small amount of HMB itself. At present, the monohydrate of HMB calcium salt, usually β-hydroxy-β-methylbutyrate calcium, is sold in the health care product market. Although its metabolic mechanism in humans is not well understood, it has been suggested to counteract muscle protein breakdown during res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C59/01
CPCC07C51/285C07C51/412C07C59/01
Inventor 汤素葵
Owner JINHU SHENKAI IND
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