high quality L-proline 147-85-3

production method

1. A hydrolyzate of protein such as gelatin or casein, treated with an ion exchange resin, and then treated with a bitter acid or Reineckeatesalt to treat only the neutral amino acid moiety, only L-proline is precipitated, and finally no Water ethanol plus isopropanol is obtained by recrystallization. It is obtained by fermentation of Corynebacterium acetoacidophilum XQ-3 (selected by the Central Research Institute of Wuxi University of Light Industry) with ammonium chloride as a nitrogen source. The acid production rate is about 60g/L.
2. There are two ways to make L-valine. First, direct fermentation method, using glucose and yellow Brevibacterium mutant strain or wild strain of Corynebacterium glutamicum, L-proline obtained by microbial fermentation; Second, chemical synthesis method, using glutamic acid as raw material, and absolute ethanol Esterification occurs under sulfuric acid catalysis, and aminosulfate is released by adding triethanolamine to obtain glutamic acid-δ-ethyl ester. The glutamic acid-δ-ethyl ester is then reduced with a metal reducing agent potassium borohydride to obtain a crude valine. Finally, the crude proline is obtained by separation and purification. Small test process Esterification Weigh 147g of L-glutamic acid, put it into a three-necked flask, add 1L of absolute ethanol, stir and cool to 0 °C, then add H2SO
4 80 ml, the reaction was stirred at 0-5 ° C for 1 h, and the reaction was continued at room temperature for 1 h, and the reaction was all clear. Add triethylamine to a pH of 8-8.5 at 20 ° C, precipitate white crystals, stir at room temperature for another 1 h, cool to cool at 5 ° C, remove the crystals, wash with 95% ethanol, drain and vacuum dry. Glutamate-δ-ethyl ester was about 141 g. The temperature of 178-180 ° C, the yield of 80% -83%. [α]32D+29.
8 (C = 1 g/ml 10% HCl). Reduction In a three-necked flask, 175 g of glutamic acid-δ-ethyl ester was added, and 875 ml of distilled water was added thereto, and the mixture was stirred and cooled to 5 ° C, and then added to KBH in several portions.
4 53.9g, about 1h addition, room temperature reaction for 1h, heat preservation 50 ° C reaction for 3h. After cooling to 0 ° C, 6 mol / L HCl was added to adjust to pH 4, and the filtrate was filtered to obtain a crude L-valine aqueous solution. Separation and Purification Ion Exchange Resin-Alumina Column Chromatography Separation A crude L-valine aqueous solution was introduced into a 732-H+ type resin exchange column at a flow rate of 4 ml/min (10 g of resin was required for 1 g of acid dosing). Rinse with distilled water until neutral, then elute with 1 mol/L ammonia water, and collect the eluate containing the L-proline fraction (controlled by silica gel G thin layer chromatography). The eluate was concentrated to dryness under reduced pressure, then dissolved in a small portion of water, and then applied to a neutral alumina column and eluted with a 60% aqueous solution of ethanol (still controlled by silica gel G thin layer chromatography). The collected eluate was concentrated to dryness under reduced pressure, and then washed several times with anhydrous ethanol. After a little cold, anhydrous diethyl ether was added, and the crystals were cooled and filtered, and dried in vacuo to give L-valine. The temperature of 220-222 ° C (decomposition), the yield of about 28%. [α]24D-82.
4 (C = 1 g/ml, H2O). Pentachlorophenol precipitation desorption separation method into salt The crude valine aqueous solution was placed in a reaction flask. When heated to 50 ° C, pentachlorophenol ethanol solution (0.111 mol / 70 ml ethanol) was added dropwise, and stirred for 5 hours, then allowed to cool. To 0 ° C, the crystals were filtered, washed with a small amount of ice water, dried, and dried to give a salt, melting point 240-242 ° C, 95%. 38.4 g of double salt was poured into a three-necked flask, and 200 ml of distilled water was added thereto, and 20 ml of ammonia water was stirred at room temperature for 8 hours. After cooling to 0 ° C, the filtrate was filtered, and the filtrate was concentrated under reduced pressure. 100 ml of distilled water was added thereto, and the filtrate was filtered, and activated carbon was decolorized. . Extract with ether, separate the aqueous layer, continue to concentrate to dryness, decolorize with anhydrous ethanol several times, add a small amount of anhydrous ethanol, add 2 times of anhydrous ether, cool the crystals, filter the crystals, and dry in vacuo to obtain L-Finished product. Amplification production process Esterification 15kg of L-glutamic acid and 100L of absolute ethanol are put into a 200L reaction tank, cooled to 0 °C, and concentrated H2SO is added dropwise under stirring.
4 8.1 L, kept at 0 ° C, stirred for 1 h, and then kept at 25 ° C for 1 h. After stirring for 1 h, triethylamine was added to adjust the pH to 8.0-8.5. After stirring for 1 h, a white precipitate appeared. After cooling to 5 ° C, the precipitate was filtered, washed with 50 L of 95% ethanol, and the precipitate was dried at 50 ° C under vacuum to give L-glutamic acid-δ-ethyl ester. Reduction The obtained L-glutamic acid-δ-ethyl ester was put into a 100L reaction tank, water was added 70L, stirred and cooled to 5 ° C, and 4.3 kg of KBH4 was added in 1 hour, heated and kept at 200 ° C, stirred for 1 h, and then heated. The reaction was stirred at 50 ° C for 3-4 h, cooled to 0 ° C, adjusted to pH 4.0 with 6 mol / L HCl, and the filtrate was filtered to give a crude L-valine solution. Precipitate the crude L-valine solution into a 100L reaction tank, heat to 50 ° C, slowly add 7L 1.5mol / L pentachlorophenol ethanol solution, keep warm at 50 ° C for 5h, then cool to 0 ° C The crystals are precipitated, the crystals are filtered, and dried to obtain a double salt. Analyze and refine the double salt into a 100L reaction tank, add 20L of 3% ammonia water, stir the reaction at room temperature for 7-8h, then cool down to 0 °C, filter, wash with a small amount of ice water, drain, wash and filtrate combined, then reduce The mixture was concentrated to dryness, stirred and dissolved with 10 L of deionized water, and the filtrate was filtered, and 0.5% activated carbon was added thereto. The mixture was heated and heated at 70 ° C for 1 hour. The filtrate was filtered, cooled to 0 ° C, and extracted with an equal volume of diethyl ether to separate the aqueous layer. Concentrate to dryness under reduced pressure, add 10 L of absolute ethanol to dehydrate 3 times, drain, add 2 L of absolute ethanol and mix well, add 10 L of diethyl ether, cool to 0 ° C, remove the precipitate by filtration, vacuum ether, 80 ° C dry , get L-valine finished product.
3. Gelatin is used as a raw material to be hydrolyzed by acid and then chromatographed on an ion exchange resin column.
4. Tobacco: BU, 22; FC, 21.

use

Proline is one of the important amino acids for the synthesis of human proteins. Widely used in the food and pharmaceutical industries, it is the main intermediate for the synthesis of captopril, enalapril and other ACE inhibitors; it is one of the important raw materials for amino acid infusion. As food additives, fine chemical raw materials, chemical catalysts, etc. have been widely used.

25 kg box/bag/drums

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