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Preparation method of 2-hydroxy-4-methylthio butyric acid metal chelate

A technology of methylthiobutyric acid and metal chelates, which is applied in the field of chemical industry and can solve the problems of nutrient destruction, high viscosity, and difficulty in mixing evenly.

Active Publication Date: 2014-01-08
NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) It has a strong corrosive and pungent odor, and it is inconvenient to store, transport and use, so it is necessary to use an expensive special liquid feeding system;
[0004] (2) It is very viscous, and it is not easy to mix evenly in the feed premix;
[0005] (3) A large amount of heat is released when it comes into contact with water, causing the feed to heat up and ferment and become rancid during storage and transportation; the acidity is very high, with a pH of about 1, and it is easy to react with feed or other ingredients in the premixed feed. Nutrients cause damage
However, the production cost of this production process is higher
Specifically, in order to obtain high yield, all need purer hydrocyanic acid, and hydrocyanic acid is often excessive, and the additional rectification purification of hydrocyanic acid and excessive use all can cause the increase of cost, and the increase of this cost , especially on an industrial scale, will lead to huge economic losses; moreover, the unsuitability of the reaction system will also increase the burden of subsequent purification and separation, reducing the yield of the product

Method used

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  • Preparation method of 2-hydroxy-4-methylthio butyric acid metal chelate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The hydrocyanic acid mixed gas I from the hydrocyanic acid synthesis tower was detected. The composition of the hydrocyanic acid mixed gas I was: 8.87% hydrocyanic acid gas, 3.88% water vapor, 1.64% ammonia gas, 1.13% hydrogen gas, nitrogen gas 76.01%, oxygen 1.48%, carbon monoxide 5.67%, carbon dioxide 1.13%, methane 0.39%.

[0055] Hydrocyanic acid mixed gas I passes through a 75% sulfuric acid tower to absorb ammonia and water vapor in the mixed gas to obtain hydrocyanic acid mixed gas II. After testing, its composition is: hydrocyanic acid gas 9.35%, hydrogen gas 1.57%, Nitrogen 79.44%, Oxygen 1.71%, Carbon Monoxide 5.79%, Carbon Dioxide 1.50%, Methane 0.64%.

Embodiment 2

[0057]Pass hydrogen cyanide mixed gas II into 223.3g of 94.5% methional with a mass fraction of 223.3g, which contains 3.3g of pyridine. React under normal pressure, control the reaction temperature to 45°C, the ventilation rate to 300L / min, absorb the tail gas with sodium hydroxide, and monitor the residual amount of methionaldehyde by HPLC. When the residual amount of methionaldehyde is less than 0.5%, it is the end of the reaction, and the feeding can be stopped. A total of 270.64 g of light yellow liquid was obtained, the content of 2-hydroxy-4-methylthiobutyronitrile was 98%, and the residual hydrocyanic acid was 0.5%. Divide the obtained 2-hydroxy-4-methylthiobutyronitrile together with the reaction solution (that is, the 2-hydroxy-4-methylthiobutyronitrile reaction system) into two parts. Add 8.5g of water to one of them, store it at 3°C ​​for 120 days, no decomposition is seen; add 8.5g of water to the other, then acidify it to pH 3 with 85% sulfuric acid, and store i...

Embodiment 3

[0061] Pass hydrogen cyanide mixed gas II into 223.3g of methional with a mass fraction of 94.5%, which contains 2.2g of pyridine and 10g of water. Under 0.15MPa, the reaction temperature is controlled to be 42°C, the ventilation rate is 280L / min, the tail gas is absorbed with sodium hydroxide, and the residual amount of methional is monitored by HPLC. When the residual amount of methionaldehyde is less than 0.5%, it is the end of the reaction, and the feeding can be stopped. A total of 279.54 g of light yellow liquid was obtained, the content of 2-hydroxy-4-methylthiobutyronitrile was 98%, and the residual hydrocyanic acid was 0.07%. The obtained 2-hydroxy-4-methylthiobutyronitrile was equally divided into two together with the reaction solution. One of them was stored at 3°C ​​for 120 days without decomposition; the other was acidified with 85% sulfuric acid to pH 3 and stored at 20°C for 130 days, 2-hydroxy-4-methylthiobutyl Nitrile decomposition rate was 0.3%.

[0062] ...

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Abstract

The invention relates to a preparation method of a 2-hydroxy-4-methylthio butyric acid metal chelate. The method comprises the following steps: performing a full reaction on hydrocyanic acid mixed gas prepared from an Andrussow method and methylthio propionaldehyde under the catalytic action of an alkali so as to obtain a 2-hydroxy-4-methylthio butyronitrile reaction system; performing a hydrolytic action on the 2-hydroxy-4-methylthio butyronitrile reaction system and sulfuric acid so as to obtain 2-hydroxy-4-methylthio butyric acid; adding an aqueous medium, a metallic compound and a crystallizing agent into the 2-hydroxy-4-methylthio butyric acid; regulating a pH value to reach 5 to 7 by using the alkali; heating to reach 60 DEG C to 90 DEG C; and performing cooling crystallization, thereby obtaining a 2-hydroxy-4-methylthio butyric acid metal chelate crystal. The method is low in production cost, wherein the obtained 2-hydroxy-4-methylthio butyric acid is easy to separate and purify, so that the 2-hydroxy-4-methylthio butyric acid with the high purity and the high yield can be obtained. Thus, the 2-hydroxy-4-methylthio butyric acid metal chelate which is further prepared from the 2-hydroxy-4-methylthio butyric acid has large crystalline particles.

Description

technical field [0001] The present invention is aimed at the field of chemical engineering, and relates to a method for preparing a metal chelate of 2-hydroxy-4-methylthiobutyrate, in particular to the preparation of 2-hydroxy-4-methylthiobutyrate on the basis of 2-hydroxy-4-methylthiobutyrate. 4-Methylthiobutanoic acid metal chelate method. Background technique [0002] 2-Hydroxy-4-methylthiobutyric acid is a methionine hydroxyl analogue, which has low toxicity, low rumen degradation rate, promotes the synthesis of rumen microorganisms, saves protein in the diet, improves the production performance of dairy cows, and improves animal health. It is the most economical and effective amino acid source for animals due to its production performance and immunity, reduced ammonia emissions, less environmental pollution, simple production process, and low price. Although methionine hydroxy analogs have the above advantages and are gradually replacing some expensive amino acids in t...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/20
Inventor 吴传隆秦岭朱小莉杨帆任星宇朱丽利陈宏杨王用贵李欧
Owner NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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