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Preparation method of large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate

A technology of calcium methylthiobutyrate and methylthiobutyric acid, which is applied in the chemical industry, can solve the problems of nutrient damage, high price, and long drying time, so as to avoid emissions, save energy, and increase the total yield Effect

Active Publication Date: 2013-12-25
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, in actual production, the synthesized calcium 2-hydroxy-4-methylthiobutyrate has a small particle size, sticky filter cake, difficult dehydration, and long drying time; the production process is dusty, inconvenient to operate, and consumes a lot of energy; in addition , the produced calcium 2-hydroxy-4-methylthiobutyrate has high viscosity, low density and poor fluency, and it is difficult to fully mix with the feed, resulting in unstable feed quality and affecting the feeding effect

Method used

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  • Preparation method of large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Dilute 340.9g of 2-hydroxy-4-methylthiobutyric acid from 88% to 40% with deionized water, then add 0.015g of lactic acid, stir and heat to 60°C, keep warm for 60 minutes, add anhydrous calcium chloride solid 111 g, during the reaction, the pH of the reaction system was adjusted to 6.0 with sodium hydroxide, and the reaction was stirred at a constant temperature for 2 hours. After the reaction was completed, cool to 10°C and press filter to obtain white crystals, which were washed twice with a small amount of cold water, and then vacuum-dried to constant weight at 90°C to obtain 331.1 g of calcium 2-hydroxy-4-methylthiobutyrate with a purity of It was 98%, and the yield was 96%. Analysis results: 2-hydroxy-4-methylthiobutyric acid content 86.2%; calcium: 11.3%; water content: 0.5%; purity 98%; 140 mesh analysis sieve 85%, in the form of smooth powder with crystals Sexual luster, bulk density (g / cm) is 0.69.

[0053] Add water to the obtained 2-hydroxy-4-methylthiobutyr...

Embodiment 2

[0055] Dilute 340.9g of 2-hydroxy-4-methylthiobutyric acid from 88% to 35% with deionized water, then add 0.034g of citric acid, stir and heat to 80°C, keep warm for 30 minutes, add anhydrous calcium chloride The solid was 111 g. During the reaction, the pH of the reaction system was adjusted to 7.0 with sodium hydroxide, and the reaction was stirred at a constant temperature for 2 hours. After the reaction was completed, cool to 10°C and press filter to obtain white crystals, which were washed twice with a small amount of cold water, and then vacuum-dried to constant weight at 90°C to obtain 331.1 g of calcium 2-hydroxy-4-methylthiobutyrate with a purity of It was 98%, and the yield was 96%. Analysis results: 2-hydroxy-4-methylthiobutyric acid content 86.2%; calcium: 11.3%; water content: 0.5%; purity 98%; 140 mesh analysis sieve 84%, in the form of smooth powder with crystals Sexual luster, bulk density (g / cm) is 0.70.

[0056] Add water and the recrystallization mother li...

Embodiment 3

[0058] Dilute 340.9g of 2-hydroxy-4-methylthiobutyric acid from 88% to 60% with deionized water, then add 0.014g of hydroxymethyl cellulose, stir and heat to 70°C, keep it warm for 30 minutes, add anhydrous Calcium carbonate solid 101g, during the reaction, adjust the pH of the reaction system with sodium hydroxide to maintain at 6.0, stir and react at constant temperature for 3 hours. After the reaction was completed, cool to 10°C and press filter to obtain white crystals, which were washed twice with a small amount of cold water, and then vacuum-dried to constant weight at 90°C to obtain 331.1 g of calcium 2-hydroxy-4-methylthiobutyrate with a purity of It was 98%, and the yield was 96%. Analysis results: 2-hydroxy-4-methylthiobutyric acid content 86.2%; calcium: 11.3%; water content: 0.5%; purity 98%; 140 mesh analysis sieve 86%, in the form of smooth powder with crystals Sexual luster, bulk density (g / cm) is 0.65.

[0059] Add water and the recrystallization mother liquo...

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Abstract

The invention belongs to the field of the chemical industry, and relates to a preparation method of large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate. The preparation method of the large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate comprises the following steps that 2-hydroxy-4-(methylthio)butyric acid, a calcium compound and a crystallizing agent are arranged in an aqueous medium, the pH is adjusted to be 5-7, the temperature is 60-80DEG C, stirring and full reactions are carried out, cooling crystallization is carried out to obtain calcium 2-hydroxy-4-(methylthio)butyrate crystals, separation is carried out to obtain crystals and coarse product mother liquid, and the crystals serve as calcium 2-hydroxy-4-(methylthio)butyrate coarse products. The calcium compound is one or more of calcium salt, calcium oxide and calcium hydroxide, and the use amount of the crystallizing agent is 50ppm-3000ppm of the mass of the 2-hydroxy-4-(methylthio)butyric acid. Materials produced through the preparation method of the large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate are high in purity, dehydration is easy, drying is rapid, crystal particles obtained after drying are large, good in mobility and large in bulk density, the amount of dust is low, glossiness is high, and the materials are more applicable to fodder.

Description

technical field [0001] The invention aims at the field of chemical industry and relates to a preparation method of calcium 2-hydroxy-4-methylthiobutyrate with large particle crystal form and high bulk density. 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 the market, they still have the following problems: [0003] (1) It has a strong corrosive and pungent odor, and it is inconvenient to ...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/20
Inventor 吴传隆秦岭杨帆丁永良朱丽利任星宇陈宏杨王用贵李欧
Owner NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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