Separation and purification method for methionine hydroxy analogue synthesized through hydrolysis of cyanohydrins

A technology for the separation and purification of methionine hydroxyl groups, applied in the field of separation and purification of chemical products, can solve the problems of difficult drying, valueless, low yield, etc., to avoid recovery and loss, simple and easy method, low cost and energy consumption Effect

Inactive Publication Date: 2015-12-09
NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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AI Technical Summary

Problems solved by technology

The problem with this method is that the obtained ammonium sulfate entrains a relatively large amount of methionine hydroxy analogs, especially the ammonium sulfate obtained by separating and purifying the organic layer, the content of which has reached about 10%. Such ammonium sulfate Has an unpleasant smell, and has a certain viscosity, is difficult to dry, and is almost worthless, which also leads to a larg

Method used

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  • Separation and purification method for methionine hydroxy analogue synthesized through hydrolysis of cyanohydrins
  • Separation and purification method for methionine hydroxy analogue synthesized through hydrolysis of cyanohydrins
  • Separation and purification method for methionine hydroxy analogue synthesized through hydrolysis of cyanohydrins

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1, cyanohydrin hydrolysis method synthesis methionine hydroxyl analog

[0032] In a coolable reactor with a pH electrode and a thermometer, add 420.2g (4mol) of 99wt% methionaldehyde, adjust the pH value to 5.0~5.5 with aqueous sodium cyanide solution, and stir vigorously at 30°C. Cool, then slowly add 189g (4.2mol) of 60wt% hydrocyanic acid aqueous solution dropwise, control the reaction temperature not to exceed 40°C, and maintain the pH value of the reaction system at about 5.5 by continuously adding sodium cyanide aqueous solution during the dropping process . Hydrocyanic acid aqueous solution is added, remove cooling bath, 30 ℃ of stirring 2 hours, obtain the reaction solution 611.2g that contains 85.83wt% 2-hydroxyl-4-methylthiobutyronitrile, the reaction yield in terms of methylthiopropionaldehyde is 99.96%.

[0033] Add 339.4g (3.0mol) of 85wt% sulfuric acid aqueous solution into the reactor, and then slowly add the above-mentioned reaction soluti...

Embodiment 2

[0034] Example 2, Separation and purification of methionine hydroxyl analogs synthesized by cyanohydrin hydrolysis

[0035] Cool the hydrolyzed solution prepared in Example 1 to 40°C, and treat it with 2 mol of gaseous ammonia or ammonia water to convert the acidic ammonium bisulfate in the system into neutral ammonium sulfate, and ammonium sulfate solids are precipitated, and stand at 60°C for stratification , to obtain the organic layer I and an aqueous layer containing ammonium sulfate solids I , and its components and contents are shown in Table 1.

[0036] Table 1 Organic layer I and water layer I components and their contents

[0037]

[0038] organic layer I Processing: the organic layer I Concentrate under reduced pressure until the moisture content is 3%, and ammonium sulfate solids are precipitated. Centrifuge at 60°C and different speeds (1500~3500r / min) for 20 minutes. The upper layer liquid separated by centrifugation is an oily yellow-brown liquid. Aft...

Embodiment 3

[0043] Example 3, Separation and purification of methionine hydroxyl analogs synthesized by cyanohydrin hydrolysis

[0044] Cool the hydrolyzate prepared in Example 1 to 40°C, and treat it with 2 mol of gaseous ammonia or ammonia water to convert the acidic ammonium bisulfate in the system into neutral ammonium sulfate, and ammonium sulfate solids are precipitated, and stand at 30°C for stratification , to obtain the organic layer I and an aqueous layer containing ammonium sulfate solids I .

[0045] organic layer I Processing: the organic layer I Concentrate under reduced pressure until the water content is 1%, and ammonium sulfate solids are precipitated. Centrifuge at 25°C and 1500r / min for 20 minutes. The upper liquid separated by centrifugation is an oily yellow-brown liquid. After testing, the ammonium sulfate content is 0.2 %, the content of methionine hydroxy analogs is 98.5%, and it is diluted with water until the content of methionine hydroxy analogs is 88%, th...

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Abstract

The invention discloses a separation and purification method for methionine hydroxy analogue synthesized through hydrolysis of cyanohydrins. The method comprises the following steps: carrying out ammonification and neutralization on hydrolysate obtained by hydrolysis of 2-hydroxy-4-methylthiobutyronitrile under the action of sulfuric acid and containing the methionine hydroxy analogue, ammonium sulfate and ammonium bisulfate, allowing ammonium sulfate to be precipitated through supersaturation and carrying out layering so as to obtain an organic layer I and a water layer I containing ammonium sulfate solid; concentrating the organic layer I so as to allow ammonium sulfate solid to be precipitated, carrying out solid-liquid separation, diluting obtained liquid through addition of water so as to obtain the commercial grade methionine hydroxy analogue, mixing the precipitated ammonium sulfate solid with the water layer I containing ammonium sulfate solid, and carrying out layering so as to obtain an organic layer II and a water layer II containing the ammonium sulfate solid; and subjecting the water layer II to solid-liquid separation and drying obtained solid so as to obtain commercial grade ammonium sulfate. The method provided by the invention is simple and easily practicable and can obtain the high-quality methionine hydroxy analogue and the commercial grade ammonium sulfate, and the recovery rates of the high-quality methionine hydroxy analogue and the commercial grade ammonium sulfate are more than 99%; and in the whole process of the method, no organic solvent is used, no waste water containing salt or organic matters is discharged, and cost and energy consumption are low.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for separating and purifying chemical products. Background technique [0002] Methionine Hydroxy Analogue (MHA) is a highly acidic liquid organic acid with 12% water content and 88% active methionine hydroxyl analogue (including at least 65% of 2-hydroxy-4-methylthio Butyric acid monomer, and 2-hydroxy-4-methylthiobutyric acid dimer and polymer with a content not exceeding 23%). In poultry feeding, methionine hydroxy analogues exhibit properties similar to those of amino acids known to act as growth stimulators and thus become important additives for animal feed. [0003] One of the synthetic methods of methionine hydroxyl analogs is cyanohydrin hydrolysis, which is to react methylthiopropionaldehyde with hydrocyanic acid to obtain 2-hydroxyl-4-methylthiobutyronitrile, which is hydrated under the action of sulfuric acid to generate 2- Hydroxy-4-methylthiobutyram...

Claims

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Application Information

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IPC IPC(8): C07C323/58C07C319/20C07C319/28C01C1/246C01C1/24
CPCC07C319/20C07C319/28C07C323/52
Inventor 吴传隆范倩玉王用贵李欧胡欣金海琴
Owner NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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