Valine purification method

A purification method, valine technology, applied in chemical instruments and methods, preparation of organic compounds, ion exchange, etc., can solve problems such as low product purity, complicated methods, and expensive precipitants

Active Publication Date: 2010-08-11
肇东星湖生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is very complicated, and it is difficult to separate valine from leucine and isoleucine, and there are problems such as time-consuming, low efficiency, and high content of impurity amino acids; 2, adding hydrochloric acid to the aqueous solution containing valine In order to generate and precipitate valine hydrochloride crystals, repeat the operation [Japanese Laid-Open Patent Application (Kokai) No.16, 450 / 1981]
The yield of valine obtained by this method is reduced
3. Purify valine by reacting it with precipitating agents such as tetrachlorophthalic acid, sulfoisophthalic acid, sulfonine, etc., which selectively form compounds with valine (Japanese Patent Pubication No.25059 / 1967) the precipitating agent used in this method is expensive and industrially difficult to obtain, the resulting compound has high solubility, it is difficult to reclaim valine with high yield, and the separation of valine from the compound is relatively complicated
Chinese patent 200710021935 removes the ion exchange process and directly adopts the method of concentration and crystallization. Although the waste water discharge is greatly reduced and the yield is improved, the product has low purity and contains many impurities.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Fermentation broth 100L, valine content 40.5g / L, adjust the pH value to 4-7, slowly add the flocculant polyaluminum chloride into the fermentation broth under stirring conditions, continue to stir for 5 minutes after adding Set aside for 10-15 minutes, when the suspension condenses to form a large number of flocs and begins to settle, stir again, slowly add the coagulant aid 0.2% cationic polyacrylamide, continue to stir for 5 minutes, let stand for 2 hours, and ferment at this time The bacteria, macromolecules and other impurity molecules in the liquid condense into flocs and settle to the bottom of the fermentation liquid. The supernatant is poured out, the sediment is washed twice with water, the water is mixed with the supernatant, and diatoms are passed through. Soil pre-coated plate and frame filter press to obtain primary filtrate. Add 1% activated carbon to the primary filtrate, and keep the temperature at 60° C. and stir at 200 rpm for 1 hour, then filter to se...

Embodiment 2

[0015] Fermentation broth 300L, valine content 41g / L, adjust pH value to 4-7, under stirring condition, slowly add flocculant polyaluminum chloride into fermentation broth, after adding, continue to stir for 5 minutes, let stand After 10 to 15 minutes, when the suspension condenses to form a large number of flocs and begins to settle, stir again, slowly add the coagulant 0.2% cationic polyacrylamide, continue to stir for 5 minutes, and let it stand for 2 hours. The bacteria, macromolecules and other impurity molecules in the fermented water condense into flocs and settle to the bottom of the fermentation broth. The supernatant is poured out, the sediment is washed twice with water, the water is mixed with the supernatant, and the diatomaceous earth is passed. Pre-coated plate and frame filter press to obtain primary filtrate. Add 1% activated carbon to the primary filtrate, and keep the temperature at 60° C. and stir at 200 rpm for 1 hour, then filter to separate the activated...

Embodiment 3

[0017]Fermentation broth 1000L, valine content 40.2g / L, adjust the pH value to 4-7, under the condition of stirring, slowly add flocculant polyaluminium chloride into the fermentation broth, after adding, continue stirring for 5 minutes, static Set aside for 10-15 minutes, when the suspension condenses to form a large number of flocs and begins to settle, stir again, slowly add the coagulant aid 0.2% cationic polyacrylamide, continue to stir for 5 minutes, let stand for 2 hours, and ferment at this time The bacteria, macromolecules and other impurity molecules in the liquid condense into flocs and settle to the bottom of the fermentation liquid. The supernatant is poured out, the sediment is washed twice with water, the water is mixed with the supernatant, and diatoms are passed through. Soil pre-coated plate and frame filter press to obtain primary filtrate. Add 1% activated carbon to the primary filtrate, and keep the temperature at 60° C. and stir at 200 rpm for 1 hour, the...

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PUM

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Abstract

The invention relates to a valine purification method, which comprises the following steps: A. adding flocculating agents into valine fermentation liquid for fast precipitating solid impurities, and obtaining primary filter liquid through filtering supernatant; B. adding activated carbon into the primary filter liquid obtained in the step A, wherein the added activated carbon accounts for 1+ / -0.5weight percent of the filter liquid, carrying out stirring and decoloration at 60 + / - 5 DEG C, and then, obtaining secondary filter liquid through filtration; C. using an industrial chromatographic column for separating inorganic salt and heteroacid, and then, using a sodium filter membrane for removing pigment and small molecular impurities to obtain a clear and colorless valine solution; D. concentrating the filter liquid for crystallization to obtain crude valine products; and E. shaking a transmission belt and raising the temperature to 220 + / - 10 DEG C, and carrying out sublimation to remove alanine and isoleucine to obtain pharmaceutical grade competitive valine products. The method has the characteristics of simple operation, good selectivity, cleanness and environment protection, so the yield and the quality of the valine are obviously improved.

Description

technical field [0001] The invention relates to a method for extracting and purifying valine from fermentation broth, especially a method for extracting pharmaceutical grade valine. Background technique [0002] The production methods of L-valine include extraction method, synthesis method, fermentation method and so on. The content of L-valine in animal blood meal, silkworm chrysalis and hair hydrolyzate is relatively high. Ion exchange technology is used to separate valine from mixed amino acids. The separation efficiency is high, the extraction operation is simple, and the production cycle is short, but the cost is high and it is not suitable for Modern industrial production. The chemical synthesis method uses isobutyraldehyde as raw material, reacts with ammonia and hydrocyanic acid to generate cyanamide, then hydrolyzes to obtain DL-valine, and obtains L-valine after resolution. The chemical synthesis method has high production cost, complex reaction, many steps and m...

Claims

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Application Information

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IPC IPC(8): C07C229/08C07C227/40B01D15/08
Inventor 郑明英宁异真雷剑芬瞿东方梁健富
Owner 肇东星湖生物科技有限公司
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