Method for preparing solid 2-hydroxy-4-(methylthio) butanoic acid

A technology of methylthiobutyric acid and hydroxymethionine, which is used in the production of food, feed additives and related fine chemicals, can solve the problems of high price, storage, transportation, and inconvenient use, and achieve the effect of low cost and simple operation

Inactive Publication Date: 2012-10-03
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Liquid MHA has a strong corrosive and pungent smell, and it is inconvenient to store, transport, and use. It is necessary to use an expensive special liquid feeding system (as described in the Chinese patent document with the publication number CN1493560A)

Method used

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  • Method for preparing solid 2-hydroxy-4-(methylthio) butanoic acid
  • Method for preparing solid 2-hydroxy-4-(methylthio) butanoic acid
  • Method for preparing solid 2-hydroxy-4-(methylthio) butanoic acid

Examples

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Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of solid 2-hydroxyl-4-methylthiobutyric acid, comprising the steps of:

[0034] a. Add 3.7g of calcium hydroxide, 17.1g of hydroxymethionine, and 60mL of ethanol into a 100mL three-necked flask, and under stirring, heat the three-necked flask to 85°C, stir and reflux for 1 hour; Standby), drying to obtain calcium hydroxymethionine;

[0035] b. Add 3.38g of calcium hydroxymethionine prepared in step a, 1.0g of concentrated sulfuric acid and 49mL of ethyl acetate into a 100mL three-neck flask, stir and react at room temperature for 2 hours; separate the mixture from solid to liquid, the precipitate is calcium sulfate, collect Liquid, made hydroxymethionine solution;

[0036] c. Distill the hydroxymethionine solution prepared in step b in a water bath with a vacuum of 0.06MPa and 40°C under reduced pressure, and dry the white or light yellow solid precipitated in the solution to constant weight at 60°C to obtain solid 2 -Hydroxy-4-methylthiobutyric a...

Embodiment 2

[0042] A preparation method of solid 2-hydroxyl-4-methylthiobutyric acid, comprising the steps of:

[0043] a. Add 5g of calcium carbonate, 17.1g of hydroxymethionine, and 60mL of methanol into a 250mL three-neck flask, and under stirring, heat the three-necked flask to 85°C, stir and reflux for 1 hour; the product is filtered by suction and washed with alcohol (recover the filtrate for later use) , drying to obtain calcium hydroxymethionine;

[0044] b. Add 3.38g of calcium hydroxymethionine prepared in step a, 1.0g of concentrated sulfuric acid and 60mL of methanol into a 100mL three-neck flask, stir and react at room temperature for 0.5h; separate the mixture from solid to liquid, the precipitate is calcium sulfate, and collect the liquid , to obtain a hydroxymethionine solution;

[0045] c. The hydroxymethionine solution prepared in step b is distilled under reduced pressure in a water bath with a vacuum degree of 0.095MPa and 70°C, and the white or light yellow solid pre...

Embodiment 3

[0048] A preparation method of solid 2-hydroxyl-4-methylthiobutyric acid, comprising the steps of:

[0049] a. Add 7.67g of barium oxide, 17.1g of hydroxymethionine, and 116mL of ethanol into a 250mL three-necked flask, and under stirring, heat the three-necked flask to 90°C, stir and reflux for 6 hours; ), drying to obtain barium hydroxymethionate;

[0050] b. Add 4.36g of barium hydroxymethionine prepared in step a, 1.0g of concentrated sulfuric acid and 70mL of ethanol into a 100mL three-neck flask, stir and react at 50°C for 6h; separate the mixture from solid to liquid, the precipitate is barium sulfate, and collect the liquid , to obtain a hydroxymethionine solution;

[0051] c. The hydroxymethionine solution prepared in step b is distilled under reduced pressure in a water bath with a vacuum degree of 0.08MPa and 50°C, and the white or light yellow solid precipitated in the solution is dried to constant weight at 80°C to obtain solid 2- Hydroxy-4-methylthiobutyric aci...

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Abstract

The invention relates to a method for preparing a solid 2-hydroxy-4-(methylthio) butanoic acid, which comprises the following steps of: a. utizling a methionine hydroxy solution to prepare methionine hydroxy calcium or hydroxy methionine barium; b. mixing the methionine hydroxy calcium or hydroxy methionine barium obtained in a step a with concentrated sulfuric acid according to a stoichiometric ratio, adding a reaction medium B, reacting for 0.5-6h at a temperature of between room temperature and 50 DEG C, stirring and carrying out solid-liquid separation to obtain a methionine hydroxy solution; and c. distilling the methionine hydroxy solution obtained in a step b in a reduced pressure to remove an organic solvent, and after drying the resulting solid, obtaining the solid 2-hydroxy-4-(methylthio) butanoic acid. Compared with the traditional molecular distillation method, the method provided by the invention has the advantages of simple operation, no needs for a short range evaporator or thin film evaporator, and low cost.

Description

technical field [0001] The invention relates to a preparation method of solid 2-hydroxy-4-methylthiobutyric acid, which belongs to the technical field of food, feed additives and related fine chemicals production. Background technique [0002] 2-hydroxyl-4-methylthiobutyric acid (2-hydroxyl-4-(methylthio)butyric acid), commonly known as hydroxymethionine or methionine hydroxyl analogue (methionine hydroxy analog, referred to as MHA), it is composed of 3-methylthio Propionaldehyde (3-(methylthio)propionaldehyde) reacts with hydrocyanic acid (HCN) to generate the corresponding α-hydroxynitrile, which is prepared by sulfuric acid-catalyzed hydrolysis. In addition to the MHA monomer, the hydrolyzate also contains a considerable proportion of water, ammonium bisulfate and ammonium sulfate (as described in the Chinese patent document with the publication number CN 1186068A and the US patent document with the patent number 6008409). In order to separate the MHA monomer from the hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/20
Inventor 盖利刚姜海辉梅庆虎
Owner QILU UNIV OF TECH
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