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Method for preparing N-methylol group-D,L-calcium methionine microelement chelates by means of saponification liquid produced through D,L- methionine

A technology of trace elements and trace metal elements, which is applied in the field of chemical industry, can solve the problems of high production cost, poor stability, and low product purity, and achieve the effect of shortening the production cycle and large cost advantages

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

However, in the existing methods for preparing methionine quantitative element chelates, there are long synthesis process cycle, low yield, high production cost, low product purity and poor stability.

Method used

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  • Method for preparing N-methylol group-D,L-calcium methionine microelement chelates by means of saponification liquid produced through D,L- methionine
  • Method for preparing N-methylol group-D,L-calcium methionine microelement chelates by means of saponification liquid produced through D,L- methionine
  • Method for preparing N-methylol group-D,L-calcium methionine microelement chelates by means of saponification liquid produced through D,L- methionine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 D, L-methionine produces saponification liquid

[0037] Mix 99.5% 3-methylthiopropanal with 30% sodium cyanide aqueous solution, then add ammonium bicarbonate aqueous solution, heat to 120°C in a closed manner, and react for 20 minutes to obtain 5-(2-methylthioethyl)- Hydantoin, decolorize the 5-(2-methylthioethyl)-hydantoin with activated carbon, add sodium hydroxide for hydrolysis, and heat the hydrolysis reaction system to 130°C to 165°C until fully hydrolyzed. Obtain a saponified solution. The saponified liquid obtained by hydrolysis can be directly used in the following examples to produce N-methylol-D, L-methionine trace element chelate after being decolorized by activated carbon. Analyze the composition of the saponified solution, which consists of the following components: D, L-methionine sodium in mass percentages of 17% ± 2%, sodium carbonate in mass percentages of 11% ± 2%, and the balance being water.

[0038] 5-(2-Methylthioethyl)-hydantoin c...

Embodiment 2

[0039] Embodiment 2 N-hydroxymethyl-D, the preparation of L-methionine zinc

[0040] Get the D after the decolorization that embodiment 1 mentions, L-methionine produces 1140 grams of saponification liquid, analyze the composition of saponification liquid: D, the mass percentage composition of L-methionine sodium is 15%, and the mass percentage composition of sodium carbonate is 10% %, the balance is water.

[0041] Add 253.1 grams (1.87mol) of anhydrous zinc chloride in batches to the above-mentioned saponified solution after decolorization, heat to 90°C, keep the reaction temperature at 90°C, react for 1 hour, filter the insoluble zinc carbonate, and cool the filtrate to At 0°C, a white precipitate was obtained, which was filtered to obtain a white D, L-methionine zinc solid.

[0042] Add the D, L-methionine zinc solid obtained above to 1 times the mass of water, stir, add 100 g (1.0 mol) of 30% formaldehyde solution to the D, L-methionine zinc slurry, keep the temperature ...

Embodiment 3

[0043] Embodiment 3 N-hydroxymethyl-D, the preparation of L-methionine ferrous

[0044] Get the saponification liquid 1140 grams after the decolouring mentioned in embodiment 1, analyze the composition of saponification liquid: D, the mass percentage composition of L-sodium methionine is 15%, and the mass percentage composition of sodium carbonate is 10%, and surplus is water .

[0045] Add 352.8 grams (1.80 mol) of ferrous chloride tetrahydrate to the above-mentioned saponified solution after decolorization, heat to 90°C, protect with nitrogen, keep the reaction temperature at 90°C, react for 1 hour, filter the insoluble matter, and cool the filtrate to 0 °C, a brown precipitate was obtained, which was filtered to obtain a brown ferrous D, L-methionine solid.

[0046] Add 1 times the quality of water to the ferrous D,L-methionine solid obtained above, stir, add 100 grams (1.0mol) of 30% formaldehyde solution to the ferrous D,L-methionine slurry, keep the temperature at 20°C,...

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Abstract

The invention relates to the field of the chemical industry, in particular to a method for preparing N-methylol group-D,L-calcium methionine microelement chelates. The method is environmentally friendly and low in cost. According to the method, saponification liquid produced in the production process of D,L-methionine serves as production raw materials and reacts with trace metal element calcium salt to obtain D,L-methionine microelement chelates, the obtained D,L-methionine microelement chelates react with formaldehyde in a water medium, filtering, washing in cold water, drying and crushing are carried out after the reaction, and the powdered N-methylol group-D,L-calcium methionine microelement chelates are obtained. According to the method, high-purity D,L-methionine is needless, the N-methylol group-D,L-calcium methionine microelement chelates are directly prepared through the saponification liquid, and production cost is reduced. According to the method, the high-purity N-methylol group-D,L-calcium methionine microelement chelates are prepared, stability is high, animals can easily digest and absorb the N-methylol group-D,L-calcium methionine microelement chelates, the N-methylol group-D,L-calcium methionine microelement chelates can serve as feed additions, obtained filter liquor can be recycled, and the method is environmentally friendly.

Description

technical field [0001] The present invention is aimed at the field of chemical industry, relates to a kind of preparation method of N-methylol-D, L-methionine trace element chelate, specifically relates to utilizing the saponification liquid produced by D, L-methionine to prepare N-methylol-D, Method of L-methionine trace element chelate. Background technique [0002] The use of metal trace elements as feed additives has gone through three stages of development: the first stage, the use of inorganic salts of trace elements, mainly sulfate and its oxides, etc., but found many shortcomings in the application, such as with other nutrients Antagonism, damage to vitamins and other nutrients, low biological potency and low mixing uniformity, etc.; the second stage: In order to overcome the shortcomings of using trace element inorganic salts, people began to use trace element additives-organic acid salts. However, organometallic trace element salts also have disadvantages such as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C319/20A23K1/16
Inventor 吴传隆王用贵秦岭朱丽利杨帆任星宇陈宏杨李欧
Owner NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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