Multistage continuous crystallization method of short rod-like methionine crystals

A methionine and short rod-shaped technology, which is applied in the field of multi-stage continuous crystallization of short rod-shaped methionine crystals, can solve the problems of difficult to meet the industrial production requirements of methionine, high cost of material use, poor crystal morphology, etc. Intermediate operation steps, the effect of reducing the difference between product batches

Active Publication Date: 2019-04-12
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the refining and separation method of methionine mainly focuses on the separation and purification of methionine and inorganic salts. Patent CN104926701A discloses a process for the purification of methionine. This method uses macroporous adsorption resin to undergo adsorption and desorption processes to achieve the separation of methionine and by-product salts The purpose; patent CN104693082A discloses a method for the separation and purification of methionine by continuous chromatography, which uses the difference between the adsorption and desorption of methionine and sodium sulfate mother liquor to chromatographic materials to achieve the purpose of desalination, but these methods generally have high material use costs and high efficiency. Low and difficult to meet the needs of industrial production of large quantities of methionine
[0006] Multi-stage evaporation and concentration of methionine aqueous solution to crystallize and purify methionine is a commonly used method for the purification and separation of methionine in the industry. It is easy to operate and can be industrialized on a large scale. Subsequent granulation process, resulting in high production costs. In addition, long-term high-temperature concentration leads to thermal decomposition of methionine, resulting in dimethyl disulfide or m...

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  • Multistage continuous crystallization method of short rod-like methionine crystals
  • Multistage continuous crystallization method of short rod-like methionine crystals
  • Multistage continuous crystallization method of short rod-like methionine crystals

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Embodiment 1

[0055] In this embodiment, a method for crystallization of methionine crystals is provided, the method for crystallization of methionine crystals is as follows: figure 1 As shown, the following steps are included: four continuous crystallization tanks are connected in series. Equip a 20% methionine feed solution in a 2L dissolution tank (add 0.080kg / h DL-methionine raw material with a purity of 90%, 0.14L / h water and 0.22L / h circulating mother liquor), heat to dissolve, and control the temperature at 130°C to obtain a clarified feed liquid; pump the clarified feed liquid into the first-stage 1L crystallization tank at a flow rate of 0.36L / h (20% solution / h), and control the temperature of the crystallization tank to 80°C, the average residence time of the slurry The time is controlled at 2.0h; the slurry in the first-stage crystallization tank is pumped into the second-stage 1L crystallization tank, the temperature of the crystallization tank is controlled at 60°C, and the ave...

Embodiment 2

[0057] In this embodiment, a method for multistage continuous crystallization of short rod-shaped methionine crystals is provided. The crystallization method of said methionine crystals is as follows: figure 2 As shown, the following steps are included: three continuous crystallization tanks are connected in series. Equip a methionine feed solution with a concentration of 15% in a 5L dissolution tank (add 0.38kg / h DL-methionine raw material with a purity of 95%, 1.92L / h water and 0.48L / h circulating mother liquor), and dissolve at high temperature, temperature control to 110°C to obtain a clarified feed liquid; pump the clarified feed liquid into the first-stage 2L crystallization tank at a flow rate of 2.4L / h (60% solution / h), and control the crystallization tank temperature to 60°C, the average residence time of the slurry The time is controlled at 0.5h; the slurry in the first-stage crystallization kettle is pumped into the second-stage 2L crystallization kettle, the tempe...

Embodiment 3

[0062] In this embodiment, a method for multistage continuous crystallization of short rod-shaped methionine crystals is provided. The crystallization method of said methionine crystals is as follows: Figure 6 As shown, the following steps are included: two continuous crystallization tanks are connected in series. Prepare a methionine feed solution with a concentration of 10% in a 1L dissolution tank (add 0.060kg / h DL-methionine raw material with a purity of 90%, 0.22L / h water and 0.32L / h circulating mother liquor), heat to dissolve, and control the temperature at 80°C to obtain a clarified feed liquid; pump the clarified feed liquid into the first-stage 1L crystallization tank at a flow rate of 0.54L / h (60% solution / h), and control the temperature of the crystallization tank to 40°C, the average residence time of the slurry The time is controlled at 0.5h; the slurry in the first-stage crystallization kettle is pumped into the second-stage 1L crystallization kettle, the tempe...

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Abstract

The invention provides a multistage continuous crystallization method of short rod-like methionine crystals. The method includes: connecting a plurality of crystallizers in series; under the action ofa circulating device, dissolving a methionine raw material at 80-130DEG C; letting the dissolved feed solution enter a first stage crystallization kettle, and controlling the kettle temperature at 60-80DEG C; enabling the slurry to enter a second stage crystallization kettle, and controlling the kettle temperature at 40-60DEG C; enabling the slurry to enter a third stage crystallization kettle, and controlling the kettle temperature at 25-40DEG C; letting the slurry enter a fourth stage crystallization kettle, and controlling the kettle temperature at 15-25DEG C; letting the final slurry flowout of the crystallization kettle and enter a solid-liquid separation system, discharging the separated solid out of the system, and returning part of the mother liquor into a dissolution kettle forfurther circulation, with the circulation volume being 20-60% of the mother liquor volume. The stage number of the crystallization kettles is supposed to be optimized according to the actual situation, and the general ideal situation is 2-4 stages. The prepared methionine crystals have short rod-like crystal habit, the crystal size is uniform, the bulk density is high, the fluidity is good, the quality is stable, the operation is simple, and the production efficiency is high, therefore the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of industrial production technology of amino acids, and relates to a multistage continuous crystallization method of short rod-shaped methionine crystals. Background technique [0002] Methionine is the only sulfur-containing amino acid among the eight essential amino acids. It is one of the important components of protein in the human body and animals. It is widely used in the fields of medicine, food, feed and cosmetics, among which feed additives are the main application Huge amount. [0003] The global demand for methionine has reached 1.3 million tons per year and is increasing at a rate of 6% per year. China’s demand in 2015 also exceeded 160,000 tons. Imports, and high-quality methionine with high bulk density and good fluidity still mainly rely on imports. [0004] The production process of methionine mainly includes biological enzyme resolution method, microbial fermentation method and chemical synthesis me...

Claims

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Application Information

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IPC IPC(8): C07C319/28C07C323/58B01D9/02
CPCB01D9/0059B01D9/0063C07B2200/13C07C319/28C07C323/58
Inventor 龚俊波汤伟伟赵绍磊尹秋响侯宝红
Owner TIANJIN UNIV
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