CN105646256A - Glutamic acid extraction crystallization process - Google Patents

Glutamic acid extraction crystallization process Download PDF

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CN105646256A
CN105646256A CN201610155801.4A CN201610155801A CN105646256A CN 105646256 A CN105646256 A CN 105646256A CN 201610155801 A CN201610155801 A CN 201610155801A CN 105646256 A CN105646256 A CN 105646256A
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liquid
clear liquid
centrifuge
tropina
glutamic acid
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CN105646256B (en
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王均成
丁兆堂
张传森
卢松
张修军
李晓永
张春宇
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INNER MONGLIA FUFENG BIOLOGICAL TECHNOLOGY Co Ltd
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N1/00Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor

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Abstract

The invention belongs to the field of amino acid production, and discloses a glutamic acid extraction crystallization process, characterized by comprising the following steps: (1) separating by a disc type centrifuge, (2) separating by a horizontal screw centrifuge, (3) secondarily separating by the disc type centrifuge, (4) mixing, (5) combining, (6) concentrating, (7) performing isoelectric treatment, (8) feeding a concentrated solution, (9) cooling, (10) centrifuging by a flat plate centrifuge, (11) performing ion exchange, and (12) drying a thallus. By adopting the process, energy conservation and emission reduction are realized, and meanwhile the quality and the extraction rate of glutamic acid are ensured.

Description

A kind of extracting glutamic acid crystallization processes
Technical field
Patent of the present invention relates to a kind of extracting glutamic acid crystallization processes, belongs to amino acids production field.
Background technology
Glutamic acid, is a kind of acidic amino acid. Molecule includes two carboxyls, and chemical name is alpha-amido 1,3-propanedicarboxylic acid. Glutamic acid is that inner Suo Xun 1856 finds, for clear crystal, has delicate flavour, is slightly soluble in water, and is dissolved in hydrochloric acid solution, isoelectric point, IP 3.22. Being present in a large number in grain protein, in animal brain, content is also more. Glutamic acid protein metabolism process in vivo accounts for critical role, participates in the many important chemical reaction in animal, plant and microorganism. Monosodium glutamate is prepared by glutamic acid and is obtained.
The extraction process that glutamic acid producer domestic at present commonly uses is to wait electricity, from handing over extraction process, lower the temperature by glutami acid fermentation liquor and use sulphuric acid and from handing over height stream by the isoelectric point, IP 3.0-3.2 of the pH regulator of fermentation liquid to glutamic acid, standing sedimentation, bottom precipitation centrifugation goes out glutamic acid, supernatant sulphuric acid adjusts pH to 1.8, the glutamic acid in clear liquid is replaced with storng-acid cation exchange resin, supernatant pH to 10 is adjusted to carry out eluting with ammonia again, the Gao Liuzai sulphuric acid eluted is adjusted to pH to 1.5, return for waiting electricity to regulate pH, from handing over workshop upper column clear liquid and washing post water and be delivered to sewage treatment plant and process, in waste water, add flocculant flocculate albumen, clear liquid after removing protein after concentration again slurry-spraying pelletizing make into fertilizer, the condensed water that concentration and evaporation goes out enters Aerobic Pond and processes. but this technique has the drawbacks such as sewage quantity is big and intractability is high, albumen quality is poor, product quality is low, soda acid consumption is big.
This outer portion producer adopts the galvanic process such as continuous concentration, after being concentrated by glutami acid fermentation liquor, temperature controls at 42-45 DEG C, stream is added to waiting in electricity tank, with the electricity tank pH such as sulphuric acid control about 3.2, crystallization draws cold cooling drawing after terminating in cold tank, use centrifuge glutamic acid, centrifugal clear liquid is discharged into sewage treatment plant, the sewage that this technique produces is few, it does not have from skill of handing over, but the yield of glutamic acid and quality are low.
Summary of the invention
In order to solve above-mentioned technical problem, the present invention provides a kind of extracting glutamic acid crystallization processes, both can guarantee that glutamic acid quality, and improved extract yield, has improved albumen quality, moreover it is possible to has reduced wastewater flow rate.
This law invention is achieved in that a kind of extracting glutamic acid crystallization processes, and it comprises the steps: 1) disc centrifuge separation, 2) horizontal screw centrifuge separation, 3) disc centrifuge secondary separation, 4) mixing, 5) merge, 6) concentration, 7) electricity such as, 8) stream adds concentrated solution, 9) cooling, 10) plate centrifuge is centrifuged, 11) ion exchange, 12) dry thalline;
Specifically, comprise the steps:
1) disc centrifuge separates: glutami acid fermentation liquor disc centrifuge is easily separated, it is centrifuged into two parts, a part is the clear liquid A containing trace tropina, tropina content 0.1%(volume ratio), another part is the protein liquid B containing a large amount of tropinas, tropina content 82%(volume ratio);
2) horizontal screw centrifuge separates: the protein liquid B horizontal screw centrifuge containing a large amount of tropinas separates, it is centrifuged into two parts, a part is the clear liquid C containing a small amount of tropina, tropina content 0.45%(volume ratio), another part is albumen underflow D in the pasty state, and albumen dry matter content is 35%(mass ratio);
3) disc centrifuge secondary separation: with disc centrifuge separating step 2) gained clear liquid C, it is divided into two parts, a part is the clear liquid E containing trace tropina, tropina content is 0.1%(volume ratio), another part is the protein liquid F containing a large amount of tropinas, and protein content is 80%(volume ratio);
4) mixing: step 3) gained protein liquid F carries out step 2 after mixing with the protein liquid containing a large amount of tropinas of the step 1) of next group feed liquid) operation;
5) merging: the clear liquid E that clear liquid A step 1) obtained and step 3) obtain merges, and is then divided into clear liquid G and clear liquid H two parts, clear liquid G is for step 6) operation, and clear liquid H is for step 7) operation; The volume ratio of clear liquid G and clear liquid H is 1:1 to 3:2;
6) concentration: adopt plate-type evaporator concentration step 5) gained clear liquid G, thickening temperature is 80 DEG C, and vacuum, at 0.06MPa, concentrates 2 times, obtains concentrated solution I;
7) electricity such as: the pH value of clear liquid H step 5) reserved with sulphuric acid is adjusted to glutamic acid isoelectric point, IP 3.2, reduces material liquid pH value 0.1-0.2 per hour, and feed liquid is progressively heated up, programming rate 2-3 DEG C/h, feed temperature rises to 40 DEG C, maintains this temperature, and this feed liquid uses as female tank feed liquid;
8) stream adds concentrated solution: in female tank feed liquid of step 7), stream adds the concentrated solution I that step 6) obtains, and is simultaneously introduced sulphuric acid, maintains pH3.2 in tank, temperature 40 DEG C; When material liquid volume accounts for the 90%-95% of tank body capacity, release the feed liquid that tank holds the 10%-15% of volume from bottom;
9) cooling: feed liquid cooling step 8) released is rapidly cooled to less than 15 DEG C;
10) plate centrifuge is centrifuged: adopting plate centrifuge to be centrifuged the feed liquid of step 9), rotating speed is 1000r/min, and glutamic acid crystal is separated by centrifugation time 10min with clear liquid J;
11) ion exchange: the isolated clear liquid J sulphuric acid of step 10) adjusts pH to 1.5, is replaced by cation exchange resin, and uses ammonia eluting, and the high flow liquid K under eluting can be used for the pH of the electricity tanks such as step 8) adjustment;
12) thalline is dried: by step 2) the albumen underflow D drying plant that obtains carries out drying to obtain tropina powder.
The technology of the present invention adopts above-mentioned technique, compares with conventional technology, has an advantage in that:
1, fermentation liquor disc centrifuge centrifugal after clear liquid the electricity such as be used for and extract glutamic acid, in waiting electric process, reduce the tropina impact on glutamic acid crystallization process, improve the quality of glutamic acid.
2, the glu thalline protein that the albumen underflow being centrifuged out through horizontal screw centrifuge obtains after drying is without any additive, purity height, quality better;
3, remove the feed liquid after albumen to cross from handing over post, reduce the impurity impact on resin, improve the adsorption rate of resin, and solve the electricity clear liquids such as continuous concentration and can not carry out from the defect handed over.
4, the clear liquid that disc centrifuge is centrifuged out is after concentration, supernatant cumulative volume reduces to original 40% ~ 50%, from after handing in waste liquid contained glutamic acid total amount than etc. ionization skill of handing over decline more than 50%, decline 80% than electricity waste liquid glutamic acid total amounts such as direct concentrations, improve the total recovery of glutamic acid.
5, the clear liquid that disc centrifuge is centrifuged out is after concentrating, and supernatant cumulative volume reduces to original 40% ~ 50%, ionizes, from the soda acid amount ratio etc. handed over, skill of handing over and declines more than 50%.
6., through above-mentioned technique, the purity of glutamic acid of the present invention can reach 97%(mass ratio) more than, clear liquid Glutamic Acid content 1.6-2.6g/100mL.
Detailed description of the invention
Hereinafter the present invention is further explained by employing specific embodiment, but should not be construed as the restriction to the new spirit of the invention.
Example one
A kind of extracting glutamic acid crystallization processes, it comprises the steps:
1) disc centrifuge separates: glutami acid fermentation liquor disc centrifuge is easily separated, it is centrifuged into two parts, a part is the clear liquid A6000L containing trace tropina, tropina content 0.1%(volume ratio), another part is the protein liquid B1500L containing a large amount of tropinas, tropina content 82%(volume ratio);
2) horizontal screw centrifuge separates: the protein liquid B1500L horizontal screw centrifuge containing a large amount of tropinas separates, it is centrifuged into two parts, a part is the clear liquid C1135L containing a small amount of tropina, tropina content 0.45%(volume ratio), another part is albumen underflow D389kg in the pasty state, and albumen dry matter content is 35%(mass ratio);
3) disc centrifuge secondary separation: with disc centrifuge separating step 2) gained clear liquid C1135L, it is divided into two parts, a part is the clear liquid E908L containing trace tropina, tropina content is 0.1%(volume ratio), another part is the protein liquid F227L containing a large amount of tropinas, and protein content is 80%(volume ratio);
4) mixing: step 3) gained tropina liquid F227L carries out step 2 after mixing with the protein liquid containing a large amount of tropinas of the step 1) of next group feed liquid) operation;
5) merging: the clear liquid E908L that clear liquid A6000L step 1) obtained and step 3) obtain merges 6908L altogether, wherein take 3908L clear liquid G and operate for step 6), the clear liquid H of 3000L is for step 7) operation;
6) concentration: with concentrator concentration step 5) the 3908L clear liquid G that obtains, employing plate-type evaporator, thickening temperature is 80 DEG C, and vacuum, at 0.06MPa, concentrates 2 times, obtains concentrated solution I1954L;
7) electricity such as: the pH value of 3000L clear liquid H step 5) reserved with sulphuric acid is adjusted to glutamic acid isoelectric point, IP 3.2, reducing material liquid pH value per hour is 0.1-0.2, and feed liquid is progressively heated up, programming rate 2-3 DEG C/h, feed temperature rises to 40 DEG C, maintaining this temperature, temperature adjusting deviation amplitude is at 1 DEG C, and this feed liquid uses as female tank feed liquid;
8) stream adds concentrated solution: in female tank feed liquid of step 7), stream adds concentrated solution I and 98% sulphuric acid that step 6) obtains, and maintains pH3.2 in tank, temperature 40 DEG C, and pH value adjusting deviation amplitude is 0.1, and temperature adjusting deviation amplitude is at 1 DEG C; When material liquid volume accounts for the 90%-95% of tank body capacity, release the feed liquid that tank holds the 10%-15% of volume from bottom, 80% that in tank, feed liquid cumulative volume must not hold less than tank;
9) cooling: feed liquid cooling step 8) released is rapidly cooled to less than 15 DEG C;
10) plate centrifuge is centrifuged: adopting plate centrifuge to be centrifuged the feed liquid of step 9), rotating speed is 1000r/min, and glutamic acid crystal is separated by centrifugation time 10min with clear liquid J; Purity can reach 97.6%;
11) ion exchange: the isolated clear liquid J of step 10) adjusts pH to 1.5 with 98% sulphuric acid, is replaced by cation exchange resin, and uses ammonia eluting, the high flow liquid K under eluting can be used for the pH of the electricity tanks such as step 8) adjustment;
12) thalline is dried: by step 2) the albumen underflow D drying plant that obtains carries out drying to obtain tropina powder 160kg, drying plant adopts revolving roll drying machine and rotary cooler, dryer entrance temperature is 600 DEG C, drop temperature is 100 DEG C, after discharging, albumen enters cooler, the drop temperature of cooler is 40 DEG C, and after drying, dried albumen moisture is 9.0%.
Finally, in addition it is also necessary to be only one of them specific embodiment of the present invention it is noted that listed above. It is clear that the invention is not restricted to above example, it is also possible to there are many deformation. All deformation that those of ordinary skill in the art can directly derive from present disclosure or associate, are all considered as protection scope of the present invention.

Claims (4)

1. an extracting glutamic acid crystallization processes, it is characterised in that described technique comprises the steps: 1) disc centrifuge separation, 2) horizontal screw centrifuge separates, and 3) disc centrifuge secondary separation, 4) mixing, 5) merge, 6) electricity such as concentration, 7), 8) stream adds concentrated solution, 9) cooling, 10) plate centrifuge is centrifuged, and 11) ion exchange, 12) dry thalline.
2. technique according to claim 1, it is characterised in that described technique comprises the steps:
1) disc centrifuge separates: glutami acid fermentation liquor disc centrifuge is easily separated, it is centrifuged into two parts, a part is the clear liquid A containing trace tropina, tropina content 0.1%(volume ratio), another part is the protein liquid B containing a large amount of tropinas, tropina content 82%(volume ratio);
2) horizontal screw centrifuge separates: the protein liquid B horizontal screw centrifuge containing a large amount of tropinas separates, it is centrifuged into two parts, a part is the clear liquid C containing a small amount of tropina, tropina content 0.45%(volume ratio), another part is albumen underflow D in the pasty state, and albumen dry matter content is 35%(mass ratio);
3) disc centrifuge secondary separation: with disc centrifuge separating step 2) gained clear liquid C, it is divided into two parts, a part is the clear liquid E containing trace tropina, tropina content is 0.1%(volume ratio), another part is the protein liquid F containing a large amount of tropinas, and protein content is 80%(volume ratio);
4) mixing: step 3) gained protein liquid F carries out step 2 after mixing with the protein liquid containing a large amount of tropinas of the step 1) of next group feed liquid) operation;
5) merging: the clear liquid E that clear liquid A step 1) obtained and step 3) obtain merges, and is then divided into clear liquid G and clear liquid H two parts, clear liquid G is for step 6) operation, and clear liquid H is for step 7) operation;
6) concentration: adopt plate-type evaporator concentration step 5) gained clear liquid G, thickening temperature is 80 DEG C, and vacuum, at 0.06MPa, concentrates 2 times, obtains concentrated solution I;
7) electricity such as: with sulphuric acid, the pH value of step 5) gained clear liquid H is adjusted to glutamic acid isoelectric point, IP 3.2, reduces material liquid pH value 0.1-0.2 per hour, and feed liquid is progressively heated up, programming rate 2-3 DEG C/h, feed temperature rises to 40 DEG C, maintains this temperature, and this feed liquid uses as female tank feed liquid;
8) stream adds concentrated solution: in female tank feed liquid of step 7), stream adds the concentrated solution I of step 6), is simultaneously introduced sulphuric acid, maintains pH3.2 in tank, temperature 40 DEG C; When material liquid volume accounts for the 90%-95% of tank body capacity, release the feed liquid that tank holds the 10%-15% of volume from bottom;
9) cooling: feed liquid cooling step 8) released is rapidly cooled to less than 15 DEG C;
10) plate centrifuge is centrifuged: adopting plate centrifuge to be centrifuged the feed liquid of step 9), rotating speed is 1000r/min, and glutamic acid crystal is separated by centrifugation time 10min with clear liquid J;
11) ion exchange: the isolated clear liquid J sulphuric acid of step 10) adjusts pH to 1.5, is replaced by cation exchange resin, and uses ammonia eluting, and eluting obtains high flow liquid K;
12) thalline is dried: by step 2) the albumen underflow D drying plant that obtains carries out drying to obtain tropina powder.
3. technique according to claim 2, it is characterised in that in described step 11), high flow liquid K is for the pH of the electricity tanks such as step 8) adjustment.
4. technique according to claim 2, it is characterised in that in described step 5), the volume ratio of clear liquid G and clear liquid H is 1:1 to 3:2.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109988790A (en) * 2019-04-09 2019-07-09 卢松 The degerming and extracting method of glutami acid fermentation liquor
CN110128286A (en) * 2019-05-23 2019-08-16 内蒙古阜丰生物科技有限公司 A kind of extracting glutamic acid crystallization processes
CN110526469A (en) * 2019-09-10 2019-12-03 河北首朗新能源科技有限公司 A kind of processing of fermentation waste water and mycoprotein recovery process and system
CN110551041A (en) * 2018-05-31 2019-12-10 卢松 extraction and purification process of glutamic acid isoelectric supernatant
CN113336662A (en) * 2021-04-18 2021-09-03 呼伦贝尔东北阜丰生物科技有限公司 Process for improving extraction crystallization of threonine
CN115399466A (en) * 2022-06-29 2022-11-29 呼伦贝尔东北阜丰生物科技有限公司 Concentration and crystallization process of sodium glutamate

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110551041A (en) * 2018-05-31 2019-12-10 卢松 extraction and purification process of glutamic acid isoelectric supernatant
CN109988790A (en) * 2019-04-09 2019-07-09 卢松 The degerming and extracting method of glutami acid fermentation liquor
CN110128286A (en) * 2019-05-23 2019-08-16 内蒙古阜丰生物科技有限公司 A kind of extracting glutamic acid crystallization processes
CN110128286B (en) * 2019-05-23 2022-03-04 内蒙古阜丰生物科技有限公司 Glutamic acid extraction and crystallization process
CN110526469A (en) * 2019-09-10 2019-12-03 河北首朗新能源科技有限公司 A kind of processing of fermentation waste water and mycoprotein recovery process and system
CN113336662A (en) * 2021-04-18 2021-09-03 呼伦贝尔东北阜丰生物科技有限公司 Process for improving extraction crystallization of threonine
CN115399466A (en) * 2022-06-29 2022-11-29 呼伦贝尔东北阜丰生物科技有限公司 Concentration and crystallization process of sodium glutamate

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