A clean process for the co-production of d,l-methionine, d,l-methionine hydroxyl analogs and their calcium salts

A technology of methionine hydroxyl group and analogs, applied in the chemical industry, can solve the problems of low extraction rate, consumption of alkali, and high extraction cost, and achieve the effects of increasing extraction rate, reducing circulation volume and low cost

Active Publication Date: 2020-09-08
LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] (1) A large amount of alkali is consumed, and a large amount of low-value-added inorganic salts are produced by-product;
[0021] (2) The production process needs to evaporate a large amount of system water or generate a large amount of waste water;
[0022] (3) The amount of material and liquid circulation is large, and the accumulation of impurities in the system affects product quality;
[0023] (4) D, L-methionine products have a low extraction rate at one time and high extraction costs;

Method used

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  • A clean process for the co-production of d,l-methionine, d,l-methionine hydroxyl analogs and their calcium salts
  • A clean process for the co-production of d,l-methionine, d,l-methionine hydroxyl analogs and their calcium salts
  • A clean process for the co-production of d,l-methionine, d,l-methionine hydroxyl analogs and their calcium salts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The preparation of embodiment 1 cyanohydrin

[0059] 6mol content of 99.5% 3-methylthiopropanal is transferred to the tank or tower reactors A and B connected in series, each adding 10~50wt% industrial desalted water relative to 3-methylthiopropanal After the citric acid-sodium hydroxide buffer salt catalyst of 0.5~5wt%, pass into the Angle method hydrogen cyanide gas (HCN content 7 ~10wt%), the tail gas after the reaction enters the secondary reactor or tower B (reaction temperature 0~25°C) for further absorption reaction, the tail gas of the secondary reactor enters the tail gas treatment system, and the reaction is kept for 1~12h, and analyzed by liquid chromatography. The primary reactor obtains cyanohydrin with a conversion rate of over 99%, and the secondary reaction obtains a mixture of cyanohydrin and 3-methylthiopropionaldehyde with a conversion rate of 20-60%.

[0060] The cyanohydrin product in the primary reactor A is transferred to obtain an aqueous cyanoh...

Embodiment 2

[0061] The preparation of embodiment 2 liquid methionine

[0062] Transfer one batch of 410g cyanohydrin (mass fraction 76wt%) obtained in Example 1 into a 316 reactor, add 0.5~1 molar equivalent of cyanohydrin concentrated sulfuric acid (98wt%), and keep warm at 30~70°C for 1~5h to generate The hydration reaction of cyanohydrin, chromatographic analysis of cyanohydrin conversion is complete, add desalinated water, carry out hydrolysis reaction at 90~130°C, heat preservation reaction for 1~5h, chromatographic analysis reaction conversion is complete, add 0.5~1.2 cyanohydrin molar equivalent 30wt% ammonia water and stir Neutralize for 10-30 minutes, let stand to separate layers, extract the water phase, further concentrate the oil phase under reduced pressure and separate the ammonium sulfate precipitated therein, and finally obtain the concentrated liquid methionine solution, add water to 88-95wt%.

Embodiment 3

[0063] The preparation of embodiment 3 solid methionine

[0064] One batch of 390g cyanohydrin (mass fraction 70wt%) obtained in Example 1 was transferred to a zirconium material autoclave, and 1~1.2 cyanohydrin molar equivalents of carbon dioxide and 2~2.2 cyanohydrin molar equivalents of 20~30wt% ammonia water were added at 140 Stir at ~160°C and 0.5~1.5MPa (speed 100~200r / min) and react for 10~60min to prepare hydantoin solution. Mix the obtained hydantoin solution with 0.95~1.2 hydantoin molar equivalents of potassium ions (in the form of potassium carbonate) and 0.8~1.2 hydantoin molar equivalents of calcium hydroxide, transfer to a zirconium material autoclave, and heat at 170~200 ° C, 0.8 Stirring under ~2.0MPa (rotation speed 110~300r / min) reaction 10~60min hydrolysis to prepare hydrolyzate and calcium carbonate precipitate, suction filter to obtain calcium carbonate precipitate and hydrolyzate, hydrolyzate after stripping, bubbling, vacuum distillation, etc. Remove t...

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Abstract

The invention discloses D,L-methionine, a D,L-methionine hydroxy analogue and a calcium salt co-production cleaning process. The process comprises the following steps that 3-methylthiopropionaldehydeand hudrogen cyanide are synthetized an intermediate of 2-hydroxy-4-methyl mercapto butyronitrile; cyanhydrin is used for preparing the D,L-methionine hydroxy analogue under the effect of inorganic acid; the cyanhydrin, carbon dioxide, ammonia gas or ammonium bicarbonate react to synthesize 5-(beta-methyl mercapto ethyl) hydantoin; obtained hydantoin reacts with calcium hydroxide under the effectof hydrolysis auxiliary agents; calcium carbonate precipitates and hydrolysate are obtained through hydrolysis; the hydrolysate releases D,L-methionine through carbon dioxide; then, mother liquid is crystallized; crystallized mother liquid containing the hydrolysis auxiliary agents is reused to the hydantoin hydrolysis step to be cyclically used; calcium carbonate and the D,L-methionine hydroxy analogue react to prepare D,L-methionine hydroxy analogue calcium salt. The hydantoin is hydrolyzed in a mode of combining few hydrolysis auxiliary agents and calcium hydroxide, so that the hydantoin hydrolysis process is economic and efficient; through the co-production of the D,L-methionine hydroxy analogue and the D,L-methionine hydroxy analogue calcium salt, by-products of calcium carbonate aredigested at inside.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a cleaning process for the joint production of D,L-methionine, D,L-methionine hydroxyl analogs and calcium salts thereof. [0002] technical background [0003] Methionine (MET), also known as methionine, is an essential amino acid required by the human body. It is widely used in food and health medicine as a nutritional supplement to balance the intake of amino acids in the human body. At the same time, it is also added to animal feed as an important functional nutrient, which can effectively promote animal growth, increase lean meat percentage and shorten feeding cycle. D, L-methionine cannot be synthesized in animals and needs to be ingested from food. Natural feed raw materials such as soybean meal and corn contain a certain amount of D,L-methionine, but it is still not enough for the required intake, so it is generally necessary to add a corresponding a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/28C07C319/20C07C323/52C07D233/76
CPCC07C319/20C07C319/28C07D233/76C07C323/52
Inventor 周荣超廖常福彭启明
Owner LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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