CN101717343B - Glutamic acid crystallization method for preventing and controlling Beta-type crystal from occurring and application thereof - Google Patents

Glutamic acid crystallization method for preventing and controlling Beta-type crystal from occurring and application thereof Download PDF

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CN101717343B
CN101717343B CN2009101941637A CN200910194163A CN101717343B CN 101717343 B CN101717343 B CN 101717343B CN 2009101941637 A CN2009101941637 A CN 2009101941637A CN 200910194163 A CN200910194163 A CN 200910194163A CN 101717343 B CN101717343 B CN 101717343B
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acid
glutamic acid
glutamic
crystal
stream
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CN101717343A (en
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李平凡
邱玉美
朱晓立
张银冰
聂青玉
杨佐毅
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Chongqing Feiya Industrial Co Ltd
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Abstract

The invention discloses a glutamic acid crystallization method for preventing and controlling Beta-type crystal from occurring and application thereof. In the invention, pure Alpha-type crystal suspending liquid is prepared as a seed crystal backing material, the glutamic acid content in supernate of the crystal suspending liquid is then measured on time, and the occurrence of the Beta-type crystal is effectively stopped by utilizing the sudden change of the content and taking relevant control measures, such as culturing crystal, accelerating regulating stream, or the like in time, therefore, the extraction ratio of the glutamic acid crystal is effectively improved. The invention not only has simple operation, but also greatly reduces the occurrence possibility of the Beta-type crystal during the crystallization of the glutamic acid, effectively improves the extraction ratio of the glutamic acid crystal, and promotes the benefit increase of enterprises.

Description

A kind of glutamic acid crystallization method and application that prevents and control light bran acid to occur
Technical field
The invention belongs to field of food, particularly a kind of glutamic acid crystallization method and application that prevents and control light bran acid to occur.
Background technology
As everyone knows, glutamic acid crystallization has multiple character, under different condition, can form the glutamic acid crystallization of different crystal forms, is divided into α-type crystallization and β-type crystallization.Wherein, α-type crystallization is tiltedly square six faceted crystals, is a kind of desirable crystallization that iso-electric point is extracted, and this crystallization purity is high, and particle is big, and quality is heavy, precipitates easily, and with the mother liquor separate easily, extract yield is high.And β-type crystallization is powdery or needle-like, flakey, and crystal grain is fine, and purity is low, crystal thing gloss, and light weight, difficult deposition is separated very difficulty with mother liquor, and extract yield is low, and this kind crystallization also usually is called as " light bran is sour ".Therefore, in crystallization operation, to avoid β-type crystalline to separate out.
Traditional extraction technology of glutamic acid is to adopt the continuous extraction process of iso-electric point low temperature; This technical process is as shown in Figure 1: traditional glutamic acid fermentation is to be raw material with starch, is hydrolyzed into after the fermentable sugars such as glucose through starch, and inoculation L-glutamic acid bacillus carries out glutamic acid fermentation; The fermentation ends aminoglutaric acid concentration generally can reach 10~13g/L; Then glutami acid fermentation liquor is carried out carrier decompression multiple-effect evaporation and concentrate, being condensed into concentration is the L-glutamic acid liquid concentrator of 25~35g/l, again this part liquid concentrator is connected stream and adds α-crystal formation glutamic acid crystallization of preparing in advance (carrying out continuous iso-electric point in the suspension-s of α-GA) extracts; Stream adds and keeps 20~30 ℃ of suspension temperatures in the process; PH3.0~3.5, stream add process will note occurring beta-crystal glutamic acid crystallization (β-GA, promptly light bran acid); The feed liquid continuous overflow of stream after adding is cooled to 5~10 ℃ more step by step, and kept 15~40 hours to educating brilliant jar simultaneously, reaches to be delivered to down operation after the requirement and to separate purification.This technology is the technology that present glutamic acid fermentation factory generally adopts, and the most important thing is to control the crystalline condition that L-glutamic acid stream adds process in this flow process.But there is unstable in the control of glutamic acid crystallization at present, causes that the reason of light bran acid has a lot, such as: the influence of operation factors, fermented liquid quality, liquid glucose quality etc.A lot of enterprises can't effectively predict β-type crystalline and occur; Can not take effective control method; More be the processing again after β-type crystallization is occurred, like this to quality product, the extracting glutamic acid yield causes great negative impact; Even a lot of enterprises have to face the reduce or stop production of long period because of the appearance of light bran acid, lose huge.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome the weak point that existing glutamic acid crystallization technology is prone to light bran acid, and a kind of glutamic acid crystallization method of preventing and controlling light bran acid to occur is provided.
Another object of the present invention is to that said prevention is provided and control the application of the glutamic acid crystallization method that the acid of light bran occurs.
The object of the invention is realized through following technical proposals: a kind of glutamic acid crystallization method of preventing and controlling light bran acid to occur specifically comprises following steps:
(1) as the preparation of the α-type crystallization suspension of crystal seed bed material
1. in 20~25 ℃, pH value to the nucleus of regulating glutami acid fermentation liquor with acid occurs, and the pH value of this moment is generally 4.5~5.3, then educates brilliant 1~3h;
2. continue to regulate pH value to 3.5~4.0 of glutami acid fermentation liquor, educate brilliant 0.5~2h in 15~20 ℃ with acid;
3. then continue to regulate pH value to 3.0~3.5 of glutami acid fermentation liquor, educate the brilliant 5~15h of stirring in 15~20 ℃ with acid; 10 * 40 microscopically microscopies obtain crystal and only are α-type crystalline α-type crystallization suspension;
(2) formation of control and adjustment glutamic acid crystallization
1. be that the L-glutamic acid liquid concentrator of 25~35% (w/w) is cooled to 25~30 ℃ with aminoglutaric acid concentration, then with 5~15m 3/ h stream is added in the α-type crystallization suspension of step (1) preparation, and stream adds and keeps the pH value in the process is 3.0~3.5, and temperature is 25~30 ℃; Add the mixing solutions that every interval 0.5~2h gets after stream adds in the process at stream and carry out quiescent setting, ST 20~60min gets the detection that supernatant carries out glutamic then;
2. select next step step according to glutamic in the supernatant:
A, supernatant glutamic are below 5.0% (w/w), and (2) the 1. said condition that then continues set by step flows and adds and detect, and keeping the supernatant glutamic is 3.5~5.0% (w/w);
B, supernatant glutamic be greater than 5.0% (w/w), then stops stream and add, and keeps temperature and pH value constant, educates crystalline substance, stops to educate crystalline substance less than 5.0% to the glutamic of supernatant, and (2) 1. said condition flows and adds and detect set by step;
(3) glutamic acid solution after step (2) stream is added carries out centrifugally, obtains glutamic acid crystal.
Before the solution centrifugal after step (2) stream adds under 10 * 40 power microscopes microscopy, do not have β-GA;
The extract yield that this preparation method obtains glutamic acid crystal reaches 92%.
Acid described in the step (1) is preferably sulfuric acid; This is based on cost consideration, and sulfuric acid concentration is high, and the concentration of the vitriol oil is generally 98%, and the consumption that on producing, uses is little, and concentration of hydrochloric acid is low, and the concentration of concentrated hydrochloric acid is generally 37%, and the consumption that on producing, uses is big, and has caused the dilution of feed liquid;
Step (2) 1. described in temperature reduction way preferably through adopting plate heat exchanger, lower the temperature with cold water;
The detection of said glutamic is to adopt the Hua Boshi respirometer to measure;
Step (2) is 2. educated crystalline substance described in the B time is preferably 1~3 hour;
Said prevention and control the preparation field that glutamic acid crystallization method that the acid of light bran occurs is applied to L-glutamic acid.
The present invention has following advantage and effect with respect to prior art:
The present invention begins to control β-type crystalline and occurs from the source.The present invention is through preparing pure α-type crystallization suspension as the crystal seed bed material; Then through regularly measuring the content of the L-glutamic acid in the crystallization suspension supernatant; Utilize the unexpected variation of content; In time make corresponding control measures, effectively prevented β-type crystalline to occur, thereby improved the extraction yield of glutamic acid crystal effectively.The present invention is simple to operate, has significantly reduced the possibility that light bran acid occurs in the glutamic acid crystallization process, has improved the extraction yield of glutamic acid crystal effectively, and one time the extracting glutamic acid yield can reach about 92%, and the benefit that has promoted enterprise increases.
Description of drawings
Fig. 1 is that traditional L-glutamic acid carries disease germs and concentrates continuous iso-electric point stream process schema.
Fig. 2 is a schema of the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1:
(1) as the preparation of the α-type crystallization suspension of crystal seed bed material, as shown in Figure 2
1. in 20 ℃, pH value to the nucleus of regulating glutami acid fermentation liquor with sulfuric acid occurs, and stops the adjusting of pH value, educates brilliant 1h;
2. continue to regulate with sulfuric acid the pH value to 3.5 of glutami acid fermentation liquor, temperature keeps 15 ℃, educates brilliant 0.5h;
3. then continue to regulate with sulfuric acid the pH value to 3.0 of glutami acid fermentation liquor, temperature keeps 15 ℃, educates brilliant 5h; 10 * 40 sediments microscope inspections obtain crystal and only are α-type crystalline α-type crystallization suspension;
(2) formation of control and adjustment glutamic acid crystallization
1. the fresh glutami acid fermentation liquor of putting jar concentrates through the quadruple effect decompression evaporator, and obtaining aminoglutaric acid concentration is the L-glutamic acid liquid concentrator of 25% (w/w), adopts plate heat exchanger, with cold water the L-glutamic acid liquid concentrator is cooled to 25 ℃, then with 5m 3/ h stream is added in the α-type crystallization suspension of step (1) preparation, and stream adds and keeps the pH value in the process is 3.0, through adding a jar built-in cooling tubulation cooling with refrigerated water through stream, makes 25 ℃ of temperature maintenance; Add the mixing solutions that every interval 0.5h gets after stream adds in the process at stream and carry out quiescent setting, ST 20min gets supernatant then, carries out the detection of glutamic with the Hua Boshi respirometer;
2. recording glutamic acid crystal content is 3.5% (w/w), and (2) the 1. said condition that continues set by step flows and adds and detect;
(3) glutamic acid solution after stream is added is through 10 * 40 power microscope microscopies, no β-GA crystal; Through the horizontal helical type whizzer, separate to obtain glutamic acid crystal in the rotating speed of 3500rpm/min, extract yield is 91.6%.
Embodiment 2
(1) as the preparation of the α-type crystallization suspension of crystal seed bed material, as shown in Figure 2
1. in 25 ℃, pH value to the nucleus of regulating glutami acid fermentation liquor with sulfuric acid occurs, and stops the adjusting of pH value, educates brilliant 2h;
2. continue to regulate with sulfuric acid the pH value to 4.0 of glutami acid fermentation liquor, temperature keeps 15 ℃, educates brilliant 1h.
3. then continue to regulate with sulfuric acid the pH value to 3.5 of glutami acid fermentation liquor, temperature keeps 20 ℃, educates brilliant 10h; The 10*40 sediments microscope inspection obtains crystal and only is α-type crystalline α-type crystallization suspension;
(2) formation of control and adjustment glutamic acid crystallization
1. the fresh glutami acid fermentation liquor of putting jar concentrates through the quadruple effect decompression evaporator, and obtaining aminoglutaric acid concentration is the L-glutamic acid liquid concentrator of 30% (w/w), adopts plate heat exchanger, with cold water the L-glutamic acid liquid concentrator is cooled to 30 ℃, then with 10m 3/ h stream is added in the α-type crystallization suspension of step (1) preparation, and stream adds and keeps the pH value in the process is 3.5, through adding a jar built-in cooling tubulation cooling with refrigerated water through stream, makes 30 ℃ of temperature maintenance; Add the mixing solutions that every interval 1h gets after stream adds in the process at stream and carry out quiescent setting, ST 40min gets supernatant then, carries out the detection of glutamic with the Hua Boshi respirometer;
2. recording glutamic acid crystal content is 5% (W/W), and (2) the 1. said condition that continues set by step flows and adds and detect;
(3) glutamic acid solution after stream is added is through 10 * 40 power microscope microscopies, no β-GA crystal; Through the horizontal helical type whizzer, separate to obtain glutamic acid crystal in the rotating speed of 3500rpm/min, extract yield is 92.3%.
Embodiment 3
(1) as the preparation of the α-type crystallization suspension of crystal seed bed material, as shown in Figure 2
1. in 23 ℃, pH value to the nucleus of regulating glutami acid fermentation liquor with sulfuric acid occurs, and stops the adjusting of pH value, educates brilliant 3h;
2. continue to regulate with sulfuric acid the pH value to 4.0 of glutami acid fermentation liquor, temperature keeps 20 ℃, educates brilliant 2h.
3. then continue to regulate with sulfuric acid the pH value to 3 of glutami acid fermentation liquor, temperature keeps 15 ℃, educates brilliant 15h; The 10*40 sediments microscope inspection obtains crystal and only is α-type crystalline α-type crystallization suspension;
(2) formation of control and adjustment glutamic acid crystallization
1. the fresh glutami acid fermentation liquor of putting jar concentrates through the quadruple effect decompression evaporator, and obtaining aminoglutaric acid concentration is the L-glutamic acid liquid concentrator of 35% (w/w), adopts plate heat exchanger, with cold water the L-glutamic acid liquid concentrator is cooled to 28 ℃, then with 5m 3/ h stream is added in the α-type crystallization suspension through step (1) preparation, and stream adds and keeps the pH value in the process is 3.5, through adding a jar built-in cooling tubulation cooling with refrigerated water through stream, makes temperature for keeping 30 ℃; Add the mixing solutions that every interval 2h gets after stream adds in the process at stream and carry out quiescent setting, ST 60min gets supernatant then, carries out the detection of supernatant glutamic with the Hua Boshi respirometer;
2. recording the supernatant glutamic is 6% (w/w), stops stream and adds, and keeps temperature and pH value constant, educates brilliant 1 hour, then detects the glutamic acid crystal content of supernatant with the Hua Boshi respirometer, is 4.5%; Then with 5m 3The speed of/h continues stream and adds, and stream adds and keeps the pH value in the process is 3.5, and temperature is 25 ℃; Add the mixing solutions that every interval 1h gets after stream adds in the process at stream and carry out quiescent setting, ST 20min gets supernatant then, carries out the detection of supernatant glutamic with the Hua Boshi respirometer;
(3) glutamic acid solution after stream is added is through 10 * 40 power microscope microscopies, no β-GA crystal; Through the horizontal helical type whizzer, separate to obtain glutamic acid crystal in the rotating speed of 3500rpm/min, extract yield is 91.8%.
Embodiment 4
(1) as the preparation of the α-type crystallization suspension of crystal seed bed material, as shown in Figure 2
1. in 25 ℃, pH value to the nucleus of regulating glutami acid fermentation liquor with sulfuric acid occurs, and stops the adjusting of pH value, educates brilliant 3h;
2. continue to regulate with sulfuric acid the pH value to 4.0 of glutami acid fermentation liquor, temperature keeps 20 ℃, educates brilliant 2h.
3. then continue to regulate with sulfuric acid the pH value to 3.3 of glutami acid fermentation liquor, temperature keeps 18 ℃, educates brilliant 15h.The 10*40 sediments microscope inspection obtains crystal and only is α-type crystalline α-type crystallization suspension;
(2) formation of control and adjustment glutamic acid crystallization
1. the fresh glutami acid fermentation liquor of putting jar concentrates through the quadruple effect decompression evaporator, and obtaining aminoglutaric acid concentration is the L-glutamic acid liquid concentrator of 25% (w/w), adopts plate heat exchanger, with cold water the L-glutamic acid liquid concentrator is cooled to 30 ℃, then with 15m 3/ h stream is added in the α-type crystallization suspension through step (1) preparation, and stream adds and keeps the pH value in the process is 3.5, through adding a jar built-in cooling tubulation cooling with refrigerated water through stream, makes 28 ℃ of temperature maintenance; Add the mixing solutions that every interval 2h gets after stream adds in the process at stream and carry out quiescent setting, ST 60min gets supernatant then, carries out the detection of glutamic with the Hua Boshi respirometer;
2. recording glutamic acid crystal content is 8% (w/w), stops stream and adds, and keeps temperature and pH value constant, educates brilliant 3 hours, then detects the glutamic acid crystal content of supernatant with the Hua Boshi respirometer, is 4.8%; Then with 5m 3The speed of/h continues stream and adds, and stream adds and keeps the pH value in the process is 3.5, and temperature is 28 ℃; Add the mixing solutions that every interval 0.5h gets after stream adds in the process at stream and carry out quiescent setting, ST 20min gets supernatant then, carries out the detection of supernatant glutamic with the Hua Boshi respirometer;
(3) glutamic acid solution after stream is added is through 10 * 40 power microscope microscopies, no β-GA crystal; Through the horizontal helical type whizzer, separate to obtain glutamic acid crystal in the rotating speed of 3500rpm/min, extract yield is 92.0%.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (5)

1. one kind is prevented and controls the sour glutamic acid crystallization method that occurs of light bran, it is characterized in that: comprise following steps:
(1) as the preparation of the ɑ-type crystallization suspension of crystal seed bed material
1. in 20~25 ℃, pH value to the nucleus of regulating glutami acid fermentation liquor with acid occurs, and then educates brilliant 1~3h;
2. continue to regulate pH value to 3.5~4.0 of glutami acid fermentation liquor, educate brilliant 0.5~2h in 15~20 ℃ with acid;
3. then continue to regulate pH value to 3.0~3.5 of glutami acid fermentation liquor, educate the brilliant 5~15h of stirring in 15~20 ℃ with acid; The microscopically microscopy obtains crystal and only is ɑ-type crystalline ɑ-type crystallization suspension;
(2) formation of control and adjustment glutamic acid crystallization
1. be that the L-glutamic acid liquid concentrator of mass percent 25~35% is cooled to 25~30 ℃ with aminoglutaric acid concentration, then with 5~15m 3/ h stream is added in the ɑ-type crystallization suspension of step (1) preparation, and stream adds and keeps the pH value in the process is 3.0~3.5, and temperature is 25~30 ℃; Add in the process every interval 0.5~2h at stream and get mixing solutions and carry out quiescent setting, ST 20~60min gets the detection that supernatant carries out glutamic then;
2. select next step step according to glutamic in the supernatant:
A, supernatant glutamic are mass percent 5.0% when following, and (2) the 1. said condition that continues set by step flows and adds and detect, and keeping the supernatant glutamic is mass percent 3.5~5.0%;
B, supernatant glutamic stop stream and add during greater than mass percent 5.0%, keep temperature and pH value constant, educate crystalline substance, to the glutamic of supernatant less than stopping to educate crystalline substance at 5.0% o'clock, (2) 1. said condition flows and adds and detect set by step;
(3) glutamic acid solution after step (2) stream is added carries out centrifugally, obtains glutamic acid crystal;
Acid described in the step (1) is sulfuric acid.
2. according to the said prevention of claim 1 with control the glutamic acid crystallization method that the acid of light bran occurs, it is characterized in that: step (2) 1. described in cooling through adopting plate heat exchanger, with the cold water realization of lowering the temperature.
3. according to the said prevention of claim 1 with control the glutamic acid crystallization method that the acid of light bran occurs, it is characterized in that: the detection of said glutamic is measured through the Hua Boshi respirometer.
4. according to the said prevention of claim 1 with control the glutamic acid crystallization method that the acid of light bran occurs, it is characterized in that: step (2) 2. described in the B to educate the brilliant time be 1~3 hour.
5. each said prevention of claim 1~4 and control the preparation field that glutamic acid crystallization method that the acid of light bran occurs is applied to L-glutamic acid.
CN2009101941637A 2009-11-25 2009-11-25 Glutamic acid crystallization method for preventing and controlling Beta-type crystal from occurring and application thereof Active CN101717343B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157625A (en) * 2007-11-27 2008-04-09 江南大学 Glutamic acid closed cycle abstraction process combined with crystal transformation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157625A (en) * 2007-11-27 2008-04-09 江南大学 Glutamic acid closed cycle abstraction process combined with crystal transformation

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘仰化等.谷氨酸晶种浅识.《发酵科技通讯》.2008,第37卷(第4期),32-33. *
战宇等.氨基酸组成和调酸速率对谷氨酸结晶的影响.《食品与发酵工业》.2000,第26卷(第2期),46-49. *
李平凡等.谷氨酸结晶控制探讨.《食品与发酵工业》.2003,第29卷(第7期),104-106. *

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