CN113121376A - Preparation method of glutamic acid - Google Patents
Preparation method of glutamic acid Download PDFInfo
- Publication number
- CN113121376A CN113121376A CN202110388306.9A CN202110388306A CN113121376A CN 113121376 A CN113121376 A CN 113121376A CN 202110388306 A CN202110388306 A CN 202110388306A CN 113121376 A CN113121376 A CN 113121376A
- Authority
- CN
- China
- Prior art keywords
- glutamic acid
- crystal
- washing
- mother liquor
- isoelectric point
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a preparation method of glutamic acid, belonging to the technical field of glutamic acid production, which is characterized by comprising a crystal washing process and a crystal transferring process, wherein before three mother liquids are subjected to first crystal washing, the pH is adjusted to the isoelectric point of the glutamic acid, and the invention has the beneficial effects that: before the crystal is washed for the first time by creatively using the tertiary mother liquor, the pH value is adjusted to the isoelectric point of glutamic acid, so that the content of beta-glutamic acid crystals in the tertiary mother liquor is reduced; the alpha-glutamic acid crystal crude product is used as a crystal nucleus, so that the generation of beta-glutamic acid crystals is avoided, the crystal form is larger, and the quality of the product is improved; meanwhile, the alpha-glutamic acid crystal crude product is subjected to secondary isoelectric point, so that the material can rapidly cross the isoelectric point of the protein, the precipitation of the protein is effectively avoided, and the generation of protein impurities is reduced.
Description
The technical field is as follows:
the invention belongs to the technical field of glutamic acid production, and particularly relates to a preparation method of glutamic acid.
Background art:
the glutamic acid is mainly used for preparing monosodium glutamate, the fermentation method for preparing the glutamic acid is the most widely applied method at home and abroad at present, and the preparation process mainly comprises the following steps: saccharification of starch, seed culture, fermentation, extraction and other steps. There are many processes for extracting glutamic acid from fermentation broth.
At present, more or isoelectric point methods are adopted to extract glutamic acid, and two key problems need to be solved for industrial-scale isoelectric crystallization of glutamic acid: firstly, the crystal habit is controlled, and secondly, the grain size distribution of crystal grains is controlled.
Crystal habit: when the glutamic acid is crystallized, two different crystal habits exist, one crystal is prismatic or pyramid-shaped alpha-type crystal, the particles are coarse, the precipitation is fast, the separation is easy, and the crystal habit expected in industrial production is realized. The other is a sheet-shaped or needle-shaped beta-type crystal, which has large specific surface area, slow precipitation and difficult separation and is a crystal habit which must be avoided in industrial production.
Particle size distribution of the crystalline particles: the particle size distribution refers to the mass or volume percentage of crystalline particles of a certain diameter in a sample. Glutamic acid crystals on an industrial scale, even if all are alpha-type crystals, have a particle diameter distribution ranging from a few micrometers to thousands of micrometers, with a major particle size distribution between 50 and 300 micrometers. The smaller the particle size of the crystalline particles, the more difficult the separation, the lower the yield and the poorer the quality.
The invention discloses a glutamic acid extraction process for producing glutamic acid by a fermentation method, which is characterized in that glutamic acid fermentation liquor is sterilized, then enters an ultrafiltration membrane for ultrafiltration, and glutamic acid is extracted by an isoelectric point method.
Various mother liquids can be generated in the actual use process, the mother liquids are directly discharged at present, a large amount of glutamic acid still remains in the mother liquids, the loss of materials is caused, and the burden is brought to sewage treatment.
The invention content is as follows:
in order to solve the problems and overcome the defects of the prior art, the invention provides a preparation method of glutamic acid, which can effectively solve the problems that mother liquor is directly discharged, a large amount of glutamic acid still remains in the mother liquor, so that the loss of materials is caused, and the burden is brought to sewage treatment.
The specific technical scheme for solving the technical problems comprises the following steps: the preparation method of the glutamic acid is characterized by comprising a crystal washing procedure and a crystal transformation procedure,
the crystal washing process comprises the following steps: the primary crystal washing process is to add the obtained alpha-glutamic acid crystal crude product into the tertiary mother liquor for primary crystal washing, and separate the primary mother liquor and the alpha-glutamic acid crystal by a separator; the secondary crystal washing procedure comprises the steps of adding alpha-glutamic acid crystals obtained by primary crystal washing into the mother liquor for four times,
the crystal transformation process comprises the steps of pumping the solution of secondary crystal washing into a crystal transformation tank for crystal transformation, separating by a separator to obtain a tertiary mother solution,
and before the third mother liquor is subjected to the first crystal washing, adjusting the pH to the isoelectric point of glutamic acid.
Before the third mother solution is subjected to the first crystal washing, the pH is adjusted to the isoelectric point of the glutamic acid, and the pH of the isoelectric point of the glutamic acid is 3.0-3.4.
The separator of the crystal washing procedure is a horizontal screw separator; the separator in the crystal transfer process is a vacuum belt separator.
The alpha-glutamic acid crystal crude product is obtained by concentrating glutamic acid fermentation liquor, performing isoelectric treatment, performing cold drawing treatment and separating.
The conditions of the crystal washing process are that the solid-liquid ratio is 80-40kg:40kg, the reaction temperature is 60 ℃, the reaction time is 2h, and the crystal washing process is carried out under the stirring action.
The condition of the crystal transformation process is that the pH of the suspension containing the alpha-glutamic acid crystals is adjusted to 4.5-4.8, the temperature is raised to 70-90 ℃, and crystal transformation is carried out under the stirring condition, so as to obtain transformation mother liquor and beta-glutamic acid crystals.
The invention has the beneficial effects that:
1. according to the invention, the secondary crystal washing is separated by the separator to obtain the tertiary mother liquor for the primary crystal washing, so that a large amount of glutamic acid in the tertiary mother liquor can be recovered, the yield of the glutamic acid is improved, and the difficulty in sewage treatment is reduced;
2. before the crystal is washed for the first time by the creative tertiary mother liquor, the pH value is adjusted to the isoelectric point of glutamic acid, so that the content of beta-glutamic acid crystals in the tertiary mother liquor is reduced;
3. the tertiary mother liquor with the pH adjusted to the isoelectric point of the glutamic acid is skillfully matched with an alpha-glutamic acid crystal crude product obtained by concentrating, isoelectric treatment, cold drawing treatment and separation of glutamic acid fermentation liquor, the secondary isoelectric treatment of the alpha-glutamic acid crystal is realized after uniform adjustment, the alpha-glutamic acid crystal crude product is used as a crystal nucleus, the generation of beta-glutamic acid crystals is avoided, the crystal form is larger, and the product quality is improved; meanwhile, the alpha-glutamic acid crystal crude product is subjected to secondary isoelectric point, so that the material can quickly cross the isoelectric point of the protein, the precipitation of the protein is effectively avoided, and the generation of protein impurities is reduced;
4. after secondary separation of secondary electro-liquid obtained by the method after a crystal washing process, the extraction efficiency of glutamic acid is greatly improved, the content of glutamic acid in secondary mother liquid is reduced, and the generation of infinite circulation of glutamic acid is avoided.
The specific implementation mode is as follows:
in the description of the invention, specific details are given only to enable a full understanding of the embodiments of the invention, but it should be understood by those skilled in the art that the invention is not limited to these details for the implementation. In other instances, well-known structures and functions have not been described or shown in detail to avoid obscuring the points of the embodiments of the invention. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The specific implementation mode of the invention is as follows:
the preparation method of the glutamic acid is characterized by comprising a crystal washing procedure and a crystal transformation procedure,
the crystal washing process comprises the following steps: the primary crystal washing process is to add the obtained alpha-glutamic acid crystal crude product into the tertiary mother liquor for primary crystal washing, and separate the primary mother liquor and the alpha-glutamic acid crystal by a separator; the secondary crystal washing procedure comprises the steps of adding alpha-glutamic acid crystals obtained by primary crystal washing into the mother liquor for four times,
the crystal transformation process comprises the steps of pumping the solution of secondary crystal washing into a crystal transformation tank for crystal transformation, separating by a separator to obtain a tertiary mother solution,
and before the third mother liquor is subjected to the first crystal washing, adjusting the pH to the isoelectric point of glutamic acid.
Before the third mother solution is subjected to the first crystal washing, the pH is adjusted to the isoelectric point of the glutamic acid, and the pH of the isoelectric point of the glutamic acid is 3.0-3.4.
The separator of the crystal washing procedure is a horizontal screw separator; the separator in the crystal transfer process is a vacuum belt separator.
The alpha-glutamic acid crystal crude product is obtained by concentrating glutamic acid fermentation liquor, performing isoelectric treatment, performing cold drawing treatment and separating.
The conditions of the crystal washing process are that the solid-liquid ratio is 80-40kg:40kg, the reaction temperature is 60 ℃, the reaction time is 2h, and the crystal washing process is carried out under the stirring action.
The condition of the crystal transformation process is that the pH of the suspension containing the alpha-glutamic acid crystals is adjusted to 4.5-4.8, the temperature is raised to 70-90 ℃, and crystal transformation is carried out under the stirring condition, so as to obtain transformation mother liquor and beta-glutamic acid crystals.
In order to more intuitively show the process advantages of the invention, the method adopting the embodiment disclosed by the invention is compared with the method adopting the comparison method of the same process,
comparative example one:
the preparation method is the same as the embodiment except that: in the preparation process of the comparative example, the mother liquor of three times is not recycled, the crystal washing procedure for one time is to add clean water to the crude product of the alpha-glutamic acid crystal for the first time,
compared with the first method, the third mother liquor is directly discharged, and a large amount of glutamic acid still remains in the mother liquor, so that the loss of materials is caused, and the burden is brought to sewage treatment;
comparative example two:
the preparation method is the same as the embodiment except that: in the preparation process of the comparative example, the pH of the three mother liquors is not adjusted to the isoelectric point of glutamic acid, and the pH is 4.5-4.7;
description of the drawings:
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a diagram of the secondary separation feed material of the present invention;
FIG. 3 is a diagram of the feed material for the second separation of comparative example two; in the drawings:
table 1: effect of different Processes on glutamic acid Crystal form
As can be seen from the comparison of FIG. 1 and the data in the table, the treated solution after the first crystal washing in the comparative example has a large amount of protein, and when the sticky substances are separated by a horizontal screw separator, the sticky substances are not easy to separate, and the separated phase is turbid; thus proving that the realization of secondary isoelectric point of the alpha-glutamic acid crystal crude product can enable the material to cross the isoelectric point of protein, effectively avoiding the precipitation of the protein and reducing the generation of protein impurities;
as can be seen from the data in Table 1:
comparison of glutamic acid crystals revealed that: the crystal form of the invention is large and uniform, the crystal form of the comparative example II is not uniform, and the beta-glutamic acid crystal has smaller beta-glutamic acid crystal; therefore, the fact that the tertiary mother liquor with the pH adjusted to the isoelectric point of the glutamic acid is skillfully matched with the alpha-glutamic acid crystal crude product obtained by concentrating, isoelectric treatment, cold drawing treatment and separation of glutamic acid fermentation liquor is uniformly adjusted to realize the secondary isoelectric point of the alpha-glutamic acid crystal, the alpha-glutamic acid crystal crude product is used as a crystal nucleus, the generation of beta-glutamic acid crystals is avoided, the crystal form is larger, and the product quality is improved;
the content comparison of the secondary mother liquor glutamic acid can be known as follows: the content of glutamic acid in the secondary mother liquor generated by the invention is reduced from 8.5-9.9% to 4.5-5.2%, which proves that the extraction efficiency of glutamic acid is greatly improved, the content of glutamic acid in the secondary mother liquor is reduced and the infinite circulation of glutamic acid is avoided after the secondary separation of secondary equal electrolyte after the crystal washing process.
In summary, the following steps:
1. according to the invention, the secondary crystal washing is separated by the separator to obtain the tertiary mother liquor for the primary crystal washing, so that a large amount of glutamic acid in the tertiary mother liquor can be recovered, the yield of the glutamic acid is improved, and the difficulty in sewage treatment is reduced;
2. before the crystal is washed for the first time by the creative tertiary mother liquor, the pH is adjusted to be 3.0-3.4 of the isoelectric point of the glutamic acid, so that the content of beta-glutamic acid crystals in the tertiary mother liquor is reduced;
3. the tertiary mother liquor with the pH adjusted to the isoelectric point of the glutamic acid is skillfully matched with an alpha-glutamic acid crystal crude product obtained by concentrating, isoelectric treatment, cold drawing treatment and separation of glutamic acid fermentation liquor, the secondary isoelectric treatment of the alpha-glutamic acid crystal is realized after uniform adjustment, the alpha-glutamic acid crystal crude product is used as a crystal nucleus, the generation of beta-glutamic acid crystals is avoided, the crystal form is larger, and the product quality is improved; meanwhile, the alpha-glutamic acid crystal crude product is subjected to secondary isoelectric point, so that the material can cross the isoelectric point of protein, the precipitation of the protein is effectively avoided, and the generation of protein impurities is reduced;
4. after secondary separation of secondary electro-liquid obtained by the method after a crystal washing process, the extraction efficiency of glutamic acid is greatly improved, the content of glutamic acid in secondary mother liquid is reduced, and the generation of infinite circulation of glutamic acid is avoided.
Claims (6)
1. A preparation method of glutamic acid is characterized by comprising a crystal washing procedure and a crystal transformation procedure,
the crystal washing process comprises the following steps: the primary crystal washing process is to add the obtained alpha-glutamic acid crystal crude product into the tertiary mother liquor for primary crystal washing, and separate the primary mother liquor and the alpha-glutamic acid crystal by a separator; the secondary crystal washing procedure comprises the steps of adding alpha-glutamic acid crystals obtained by primary crystal washing into the mother liquor for four times,
the crystal transformation process comprises the steps of pumping the solution of secondary crystal washing into a crystal transformation tank for crystal transformation, separating by a separator to obtain a tertiary mother solution,
and before the third mother liquor is subjected to the first crystal washing, adjusting the pH to the isoelectric point of glutamic acid.
2. The method according to claim 1, wherein the pH of the third mother liquor is adjusted to the isoelectric point of glutamic acid before the first crystal washing, and the pH of the isoelectric point of glutamic acid is 3.0 to 3.4.
3. The method according to claim 1, wherein the separator in the crystal washing step is a horizontal screw separator; the separator in the crystal transfer process is a vacuum belt separator.
4. The method of producing glutamic acid according to claim 1, wherein the crude α -glutamic acid crystal is obtained by concentrating a glutamic acid fermentation broth, subjecting to isoelectric treatment, subjecting to cold drawing treatment, and separating.
5. The method of claim 1, wherein the step of washing the crystals is carried out under stirring at a solid-to-liquid ratio of 80-40kg to 40kg at 60 ℃ for 2 hours.
6. The method of producing glutamic acid according to claim 1, wherein the conditions of the crystal transformation step are such that a suspension containing the α -glutamic acid crystals is adjusted to pH 4.5 to 4.8, heated to 70 to 90 ℃, and subjected to crystal transformation under stirring to obtain a transformation mother liquor and β -glutamic acid crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110388306.9A CN113121376A (en) | 2021-04-12 | 2021-04-12 | Preparation method of glutamic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110388306.9A CN113121376A (en) | 2021-04-12 | 2021-04-12 | Preparation method of glutamic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113121376A true CN113121376A (en) | 2021-07-16 |
Family
ID=76776102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110388306.9A Pending CN113121376A (en) | 2021-04-12 | 2021-04-12 | Preparation method of glutamic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113121376A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB986738A (en) * | 1962-10-09 | 1965-03-24 | Ajinomoto Kk | A process for recovering crystalline glutamic acid from a glutamic acid-containing fermentation broth |
| CN1312245A (en) * | 2001-02-13 | 2001-09-12 | 盛自华 | Glutamic acid extracting process from fermentation liquid |
| CN101156675A (en) * | 2007-11-08 | 2008-04-09 | 江南大学 | Glutamic acid abstraction technics combining rotation crystal |
| CN101671705A (en) * | 2009-07-23 | 2010-03-17 | 阜新豪森生物科技有限公司 | Extraction technology of glutamic acid recovered by combining crystal transformation and ion exchange |
| CN101735088A (en) * | 2009-11-30 | 2010-06-16 | 北京坡华生物科技有限公司 | Production process of glutamic acid and monosodium glutamate |
| CN105111097A (en) * | 2015-09-14 | 2015-12-02 | 宝鸡阜丰生物科技有限公司 | Refining technology for glutamic acid |
-
2021
- 2021-04-12 CN CN202110388306.9A patent/CN113121376A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB986738A (en) * | 1962-10-09 | 1965-03-24 | Ajinomoto Kk | A process for recovering crystalline glutamic acid from a glutamic acid-containing fermentation broth |
| CN1312245A (en) * | 2001-02-13 | 2001-09-12 | 盛自华 | Glutamic acid extracting process from fermentation liquid |
| CN101156675A (en) * | 2007-11-08 | 2008-04-09 | 江南大学 | Glutamic acid abstraction technics combining rotation crystal |
| CN101671705A (en) * | 2009-07-23 | 2010-03-17 | 阜新豪森生物科技有限公司 | Extraction technology of glutamic acid recovered by combining crystal transformation and ion exchange |
| CN101735088A (en) * | 2009-11-30 | 2010-06-16 | 北京坡华生物科技有限公司 | Production process of glutamic acid and monosodium glutamate |
| CN105111097A (en) * | 2015-09-14 | 2015-12-02 | 宝鸡阜丰生物科技有限公司 | Refining technology for glutamic acid |
Non-Patent Citations (1)
| Title |
|---|
| 宋炜等: "糖蜜淀粉发酵味精处理末次味精母液的工艺研究", 《甘蔗糖业》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112574263B (en) | Preparation method of psicose crystal | |
| CN102329212A (en) | Refining method for long-chain binary acid | |
| CN112195171A (en) | Method for preparing beta-alanine by using immobilized enzyme | |
| US20230159579A1 (en) | Crystallization of allulose under reduced pressure | |
| CN103804172A (en) | Method for improving organic acid product quality | |
| WO2022247197A1 (en) | System and method for co-producing erythritol and liquid sorbitol by using corn starch | |
| CN112250722B (en) | Production process of lactitol crystal | |
| CN113121376A (en) | Preparation method of glutamic acid | |
| CN102703334B (en) | Strain producing erythritol and method for producing erythritol by using strain | |
| CN110655547A (en) | Adenosine extraction method for reducing content of single related impurities | |
| KR100864673B1 (en) | Method of recovering L-Threonine from L-Threonine fermentation broth using a nonsolvent | |
| CN113912475B (en) | Preparation method of erythritol crystals | |
| CN110408672B (en) | Method for extracting D-lactic acid from D-lactic acid waste liquid | |
| CN111808999B (en) | Sucrose seed crystal and preparation method thereof | |
| CN110606863B (en) | Preparation method of N-acetylneuraminic acid dihydrate | |
| CN111518119B (en) | Continuous amoxicillin crystallization process | |
| CN218910200U (en) | Xylitol crystal's preparation system | |
| CN113024393A (en) | Extraction system for recovering glutamic acid from desalted liquid and use method | |
| CN112552188B (en) | Preparation method of sertraline hydrochloride crystal form I | |
| CN220867438U (en) | D-mannose production device | |
| CN114478235B (en) | Method for purifying organic acid in fermentation liquor | |
| CN102367255B (en) | Method for extracting riboflavin from riboflavin fermentation liquor | |
| CN116768284B (en) | Environment-friendly process for producing cobalt sulfate | |
| CN117487876A (en) | Preparation method of 80% feed-grade riboflavin | |
| CN116444585A (en) | Refining method of D-psicose |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210716 |
|
| RJ01 | Rejection of invention patent application after publication |