CN110885862A - Preparation method of L-lysine sulfate and by-product thereof - Google Patents
Preparation method of L-lysine sulfate and by-product thereof Download PDFInfo
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- CN110885862A CN110885862A CN201910824251.4A CN201910824251A CN110885862A CN 110885862 A CN110885862 A CN 110885862A CN 201910824251 A CN201910824251 A CN 201910824251A CN 110885862 A CN110885862 A CN 110885862A
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- lysine
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- sulfate
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- VJDRZAPMMKFJEA-JEDNCBNOSA-N (2s)-2,6-diaminohexanoic acid;sulfuric acid Chemical compound OS(O)(=O)=O.NCCCC[C@H](N)C(O)=O VJDRZAPMMKFJEA-JEDNCBNOSA-N 0.000 title claims abstract description 16
- 239000006227 byproduct Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 238000000855 fermentation Methods 0.000 claims abstract description 48
- 230000004151 fermentation Effects 0.000 claims abstract description 48
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000004472 Lysine Substances 0.000 claims abstract description 44
- 235000018977 lysine Nutrition 0.000 claims abstract description 44
- 239000001963 growth medium Substances 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 17
- 238000005469 granulation Methods 0.000 claims abstract description 16
- 230000003179 granulation Effects 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 241000894006 Bacteria Species 0.000 claims abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 9
- 241001052560 Thallis Species 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 230000001954 sterilising effect Effects 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 239000007921 spray Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 12
- 241000186226 Corynebacterium glutamicum Species 0.000 claims description 9
- 244000005700 microbiome Species 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 238000011081 inoculation Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 230000004060 metabolic process Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 229960003646 lysine Drugs 0.000 description 35
- 239000011148 porous material Substances 0.000 description 5
- 235000015097 nutrients Nutrition 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- BVHLGVCQOALMSV-JEDNCBNOSA-N L-lysine hydrochloride Chemical compound Cl.NCCCC[C@H](N)C(O)=O BVHLGVCQOALMSV-JEDNCBNOSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 235000020776 essential amino acid Nutrition 0.000 description 2
- 239000003797 essential amino acid Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229960005337 lysine hydrochloride Drugs 0.000 description 2
- 208000019901 Anxiety disease Diseases 0.000 description 1
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 241000319304 [Brevibacterium] flavum Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P13/00—Preparation of nitrogen-containing organic compounds
- C12P13/04—Alpha- or beta- amino acids
- C12P13/08—Lysine; Diaminopimelic acid; Threonine; Valine
-
- 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
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- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a preparation method of L-lysine sulfate and a byproduct thereof, belonging to the technical field of lysine production process and comprising the following steps: sterilizing a culture medium; fermenting, inoculating lysine producing bacteria under sterile condition, controlling temperature at 35-40 deg.C, pH at 6.8-7.0 and DO at 20-30% during fermentation process, and fermenting for 48-60 hr; extracting and purifying, after fermentation, putting the mixture of lysine and a substrate in an isoelectric extraction workshop, adjusting the pH value of a fermentation solution to 5-6 by using sulfuric acid, filtering the treated fermentation solution by using ceramic membrane equipment to remove thalli, sticky substances and residues, performing triple-effect concentration on the filtered clear solution to obtain a concentrated solution with the concentration of 20 Baume, and performing granulation and drying by using a spray granulation bed to obtain a finished product. The invention overcomes the difficult problem of environmental protection, reduces the production links, has short process route, low consumption of raw and auxiliary materials and low cost, and has high content of produced lysine.
Description
Technical Field
The invention relates to the technical field of lysine production processes, and particularly relates to a preparation method of L-lysine sulfate and a by-product thereof.
Background
Lysine (Lysine) has the chemical name 2, 6-diaminohexanoic acid. Lysine is a basic essential amino acid. The cereal is called the first limiting amino acid because of its very low lysine content and its easy destruction and lack during processing.
Lysine is one of the essential amino acids in humans and mammals, and is not synthesized by the body itself and must be supplemented from food. Lysine is mainly present in animal foods and legumes, and lysine content in cereals is very low. Lysine has positive nutritional significance in promoting growth and development of human body, enhancing immunity of organism, resisting virus, promoting fat oxidation, relieving anxiety, promoting absorption of certain nutrients, and can act synergistically with certain nutrients to better exert physiological functions of various nutrients.
The direct fermentation method is a widely used lysine production method. The commonly used raw materials are cheap sugar raw materials such as waste molasses, starch hydrolysate and the like after sugar production of sugarcane or beet. In addition, acetic acid, ethanol, etc. are also optional raw materials. The main microorganisms for producing lysine by direct fermentation method include mutant strains of Corynebacterium glutamicum, Brevibacterium flavum and Brevibacterium lactofermentum. The method is developed in the later 50 th of the 20 th century, and since 70 s, some mutant strains with multiple genetic markers are bred due to the development of breeding technology, so that the process is mature day by day, and the yield of lysine is increased manyfold. The maximum yield of acid in industrial production is improved to 120g per liter of fermentation, and the extraction rate reaches about 80-90%.
Lysine, one of the feed additive materials, plays an extremely important role in feed formulation and nutrient supply. At present, 98 lysine hydrochloride and 70 lysine sulfate are taken as main components in lysine products in markets at home and abroad. 98 lysine hydrochloride, which is produced by ion exchange, has great environmental pollution and high production cost.
Disclosure of Invention
The invention provides a preparation method of L-lysine sulfate and a byproduct thereof, which solves the problems of great environmental pollution and high production cost of the existing direct fermentation production process.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a method for preparing L-lysine sulfate and by-products thereof comprises the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using steam to cause microorganism death;
(2) fermentation: inoculating lysine producing bacteria under aseptic condition, controlling temperature at 35-40 deg.C, pH at 6.8-7.0 and DO at 20-30% during fermentation, and fermenting for 48-60 hr to maximally accumulate lysine in the metabolic process;
(3) extraction and purification: after fermentation, putting the mixture of lysine and substrate in an isoelectric extraction workshop, adjusting the pH value of fermentation liquid to 5-6 by using sulfuric acid, filtering the treated fermentation liquid by ceramic membrane equipment to remove bacteria, viscous substances and residues, performing triple-effect concentration on the filtered clear liquid to obtain concentrated liquid with the concentration of 20 Baume, and performing granulation drying by using a spray granulation bed to obtain a finished product.
Wherein, the temperature of the steam in the step (1) is preferably 120-130 ℃.
Among them, preferably, the lysine-producing bacterium is Corynebacterium glutamicum.
Wherein, the inoculation amount of the lysine-producing bacteria is preferably 15-18% of the weight of the culture medium.
Wherein, preferably: the aperture of the ceramic membrane is 50 nm.
Compared with the prior art, the technical scheme of the invention has the following obvious effects:
in the extraction and purification process, after the pH value is adjusted by sulfuric acid, a ceramic membrane device is adopted for filtering to remove thalli, sticky substances and residues, and the filtered clear solution is subjected to triple-effect concentration.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example provides a method for preparing L-lysine sulfate and its by-products, comprising the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using steam at 125 ℃ to cause the death of microorganisms, wherein the heating time is 30 min;
(2) fermentation: inoculating corynebacterium glutamicum in an aseptic state, wherein the inoculation amount is 16% of the weight of a culture medium, the fermentation process is controlled at the temperature of 38 ℃, the pH value is 6.9, the DO value is 25%, and the fermentation time is 55 hours, so that lysine is accumulated in lysine producing bacteria to the maximum extent through a metabolic process;
(3) extraction and purification: after fermentation, putting the mixture of lysine and substrate in an isoelectric extraction workshop, adjusting the pH value of the fermentation solution to 5.5 by using sulfuric acid, filtering the treated fermentation solution by using a ceramic membrane device with the pore diameter of 50nm to remove thalli, sticky substances and residues, performing triple-effect concentration on the filtered clear solution to obtain a concentrated solution with the concentration of 20 Baume, and performing granulation drying by using a spray granulation bed to obtain a finished product.
Example 2
This example provides a method for preparing L-lysine sulfate and its by-products, comprising the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using 120 ℃ steam to cause the death of microorganisms, wherein the heating time is 30 min;
(2) fermentation: inoculating corynebacterium glutamicum in an aseptic state, wherein the inoculation amount is 18 percent of the weight of a culture medium, the temperature is controlled at 35 ℃ in the fermentation process, the pH value is 20 percent, the fermentation time is 60 hours, and lysine is accumulated in lysine producing bacteria to the maximum extent through the metabolic process;
(3) extraction and purification: after the fermentation is finished, putting the mixture of lysine and a substrate in an isoelectric extraction workshop, adjusting the pH value of a fermentation solution to 5 by using sulfuric acid, filtering the treated fermentation solution by using ceramic membrane equipment with the pore diameter of 50nm to remove thalli, sticky substances and residues, performing triple-effect concentration on the filtered clear solution to obtain a concentrated solution with the concentration of 20 Baume, and performing granulation drying by using a spray granulation bed to obtain a finished product.
Example 3
This example provides a method for preparing L-lysine sulfate and its by-products, comprising the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using 130 ℃ steam to cause the death of microorganisms, wherein the heating time is 30 min;
(2) fermentation: inoculating corynebacterium glutamicum in an aseptic state, wherein the inoculation amount is 15% of the weight of a culture medium, the temperature is controlled to be 40 ℃, the pH value is 6.8, the DO value is 30% in the fermentation process, and the fermentation time is 48 hours, so that lysine is accumulated in lysine producing bacteria to the maximum extent through the metabolic process;
(3) extraction and purification: after the fermentation is finished, putting the mixture of lysine and a substrate in an isoelectric extraction workshop, adjusting the pH value of a fermentation solution to 6 by using sulfuric acid, filtering the treated fermentation solution by using ceramic membrane equipment with the pore diameter of 50nm to remove thalli, sticky substances and residues, performing triple-effect concentration on the filtered clear solution to obtain a concentrated solution with the concentration of 20 Baume, and performing granulation drying by using a spray granulation bed to obtain a finished product.
Example 4
This example provides a method for preparing L-lysine sulfate and its by-products, comprising the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using 130 ℃ steam to cause the death of microorganisms, wherein the heating time is 30 min;
(2) fermentation: inoculating corynebacterium glutamicum in an aseptic state, wherein the inoculation amount is 17% of the weight of a culture medium, the fermentation process is controlled at the temperature of 38 ℃, the pH value is 6.9, the DO value is 22%, and the fermentation time is 50 hours, so that lysine is accumulated in lysine producing bacteria to the maximum extent through a metabolic process;
(3) extraction and purification: after fermentation, putting the mixture of lysine and substrate in an isoelectric extraction workshop, adjusting the pH value of the fermentation solution to 5.8 by using sulfuric acid, filtering the treated fermentation solution by using a ceramic membrane device with the pore diameter of 50nm to remove thalli, sticky substances and residues, performing triple-effect concentration on the filtered clear solution to obtain a concentrated solution with the concentration of 20 Baume, and performing granulation drying by using a spray granulation bed to obtain a finished product.
Example 5
This example provides a method for preparing L-lysine sulfate and its by-products, comprising the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using 120 ℃ steam to cause the death of microorganisms, wherein the heating time is 30 min;
(2) fermentation: inoculating corynebacterium glutamicum in an aseptic state, wherein the inoculation amount is 17% of the weight of a culture medium, the fermentation process is controlled at 38 ℃, the pH value is 6.9, the DO value is 28%, and the fermentation time is 48-60 hours, so that lysine is accumulated in lysine producing bacteria to the maximum extent through the metabolic process;
(3) extraction and purification: after the fermentation is finished, the mixture of lysine and a substrate is placed in an isoelectric extraction workshop, the pH value of the fermentation solution is adjusted to 5.9 by sulfuric acid, the treated fermentation solution is filtered by a ceramic membrane device with the pore diameter of 50nm to remove thalli, sticky substances and slag substances, the filtered clear solution is subjected to triple-effect concentration to obtain a concentrated solution with the concentration of 20 Baume, and a spraying granulation bed is used for granulation and drying to obtain a finished product.
The performance indicators obtained in examples 1-5 were examined and the results were as follows: a
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing L-lysine sulfate and by-products thereof is characterized by comprising the following steps:
(1) and (3) sterilizing a culture medium: continuously heating the culture medium by using steam so as to kill microorganisms;
(2) fermentation: inoculating lysine producing bacteria under aseptic condition, controlling temperature at 35-40 deg.C, pH at 6.8-7.0 and DO at 20-30% during fermentation, and fermenting for 48-60 hr to maximally accumulate lysine in the metabolic process;
(3) extraction and purification: after fermentation, putting the mixture of lysine and substrate in an isoelectric extraction workshop, adjusting the pH value of fermentation liquid to 5-6 by using sulfuric acid, filtering the treated fermentation liquid by ceramic membrane equipment to remove thalli, sticky substances and residues, performing triple-effect concentration on the filtered clear liquid to obtain a concentrated solution with the concentration of 20 Baume, and performing granulation drying by using a spray granulation bed to obtain a finished product.
2. The method for preparing L-lysine sulfate and its by-products according to claim 1, wherein: the temperature of the steam in the step (1) is 120-130 ℃.
3. The method for preparing L-lysine sulfate and its by-products according to claim 1, wherein: the lysine producing strain is Corynebacterium glutamicum.
4. The method of claim 3 for preparing L-lysine sulfate and its by-products, comprising: the inoculation amount of the lysine producing bacteria is 15-18% of the weight of the culture medium.
5. The method for preparing L-lysine sulfate and its by-products according to claim 1, wherein: the aperture of the ceramic membrane is 50 nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910824251.4A CN110885862A (en) | 2019-09-02 | 2019-09-02 | Preparation method of L-lysine sulfate and by-product thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910824251.4A CN110885862A (en) | 2019-09-02 | 2019-09-02 | Preparation method of L-lysine sulfate and by-product thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5133976A (en) * | 1983-03-03 | 1992-07-28 | Rhone-Poulenc Sante | Fermentation process for producing lysine sulphate for animal nutrition |
| CN103553951A (en) * | 2013-10-31 | 2014-02-05 | 安徽丰原发酵技术工程研究有限公司 | Method of extracting and preparing lysine sulphate from fermenting liquid containing lysin |
| CN104276967A (en) * | 2013-07-01 | 2015-01-14 | 中粮生物化学（安徽）股份有限公司 | Method for producing low-lysine -content product |
| CN106755156A (en) * | 2016-12-28 | 2017-05-31 | 安徽丰原发酵技术工程研究有限公司 | A kind of fermentation process of L lysines |
-
2019
- 2019-09-02 CN CN201910824251.4A patent/CN110885862A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5133976A (en) * | 1983-03-03 | 1992-07-28 | Rhone-Poulenc Sante | Fermentation process for producing lysine sulphate for animal nutrition |
| CN104276967A (en) * | 2013-07-01 | 2015-01-14 | 中粮生物化学（安徽）股份有限公司 | Method for producing low-lysine -content product |
| CN103553951A (en) * | 2013-10-31 | 2014-02-05 | 安徽丰原发酵技术工程研究有限公司 | Method of extracting and preparing lysine sulphate from fermenting liquid containing lysin |
| CN106755156A (en) * | 2016-12-28 | 2017-05-31 | 安徽丰原发酵技术工程研究有限公司 | A kind of fermentation process of L lysines |
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Application publication date: 20200317 |