CN113249412A - Preparation method of fermentation source calcium propionate - Google Patents
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- CN113249412A CN113249412A CN202110540013.8A CN202110540013A CN113249412A CN 113249412 A CN113249412 A CN 113249412A CN 202110540013 A CN202110540013 A CN 202110540013A CN 113249412 A CN113249412 A CN 113249412A
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- 238000000855 fermentation Methods 0.000 title claims abstract description 50
- 230000004151 fermentation Effects 0.000 title claims abstract description 47
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 title claims abstract description 32
- 235000010331 calcium propionate Nutrition 0.000 title claims abstract description 32
- 239000004330 calcium propionate Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000007788 liquid Substances 0.000 claims abstract description 41
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims abstract description 33
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- NVNLLIYOARQCIX-MSHCCFNRSA-N Nisin Chemical compound N1C(=O)[C@@H](CC(C)C)NC(=O)C(=C)NC(=O)[C@@H]([C@H](C)CC)NC(=O)[C@@H](NC(=O)C(=C/C)/NC(=O)[C@H](N)[C@H](C)CC)CSC[C@@H]1C(=O)N[C@@H]1C(=O)N2CCC[C@@H]2C(=O)NCC(=O)N[C@@H](C(=O)N[C@H](CCCCN)C(=O)N[C@@H]2C(NCC(=O)N[C@H](C)C(=O)N[C@H](CC(C)C)C(=O)N[C@H](CCSC)C(=O)NCC(=O)N[C@H](CS[C@@H]2C)C(=O)N[C@H](CC(N)=O)C(=O)N[C@H](CCSC)C(=O)N[C@H](CCCCN)C(=O)N[C@@H]2C(N[C@H](C)C(=O)N[C@@H]3C(=O)N[C@@H](C(N[C@H](CC=4NC=NC=4)C(=O)N[C@H](CS[C@@H]3C)C(=O)N[C@H](CO)C(=O)N[C@H]([C@H](C)CC)C(=O)N[C@H](CC=3NC=NC=3)C(=O)N[C@H](C(C)C)C(=O)NC(=C)C(=O)N[C@H](CCCCN)C(O)=O)=O)CS[C@@H]2C)=O)=O)CS[C@@H]1C NVNLLIYOARQCIX-MSHCCFNRSA-N 0.000 claims abstract description 14
- 108010053775 Nisin Proteins 0.000 claims abstract description 14
- 239000004309 nisin Substances 0.000 claims abstract description 14
- 235000010297 nisin Nutrition 0.000 claims abstract description 14
- 239000001963 growth medium Substances 0.000 claims abstract description 12
- 239000002699 waste material Substances 0.000 claims abstract description 12
- 241000894006 Bacteria Species 0.000 claims abstract description 11
- 239000007791 liquid phase Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000002921 fermentation waste Substances 0.000 claims abstract description 9
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims abstract description 7
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 7
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 7
- 230000001954 sterilising effect Effects 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 32
- 239000004310 lactic acid Substances 0.000 claims description 16
- 235000014655 lactic acid Nutrition 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 238000005374 membrane filtration Methods 0.000 claims description 6
- 241000186428 Propionibacterium freudenreichii Species 0.000 claims description 5
- 241000186429 Propionibacterium Species 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000012510 hollow fiber Substances 0.000 claims description 3
- 238000011081 inoculation Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000002308 calcification Effects 0.000 abstract description 3
- 235000019249 food preservative Nutrition 0.000 abstract description 2
- 239000005452 food preservative Substances 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract 1
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000008929 regeneration Effects 0.000 abstract 1
- 238000011069 regeneration method Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 5
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 5
- 235000010334 sodium propionate Nutrition 0.000 description 5
- 239000004324 sodium propionate Substances 0.000 description 5
- 229960003212 sodium propionate Drugs 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 241001052560 Thallis Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- -1 bacteria Natural products 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
- C12P7/52—Propionic acid; Butyric acids
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, 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
- C12N1/20—Bacteria; Culture media therefor
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- Wood Science & Technology (AREA)
- Genetics & Genomics (AREA)
- Biotechnology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
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- Virology (AREA)
- Tropical Medicine & Parasitology (AREA)
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- General Chemical & Material Sciences (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a preparation method of fermentation source calcium propionate, and belongs to the technical field of biological food preservatives. The method comprises the following steps: 1) taking nisin fermentation waste liquid as a culture medium, sterilizing, inoculating propionic acid bacteria, performing secondary fermentation at 30 ℃ under an anaerobic condition, and maintaining the pH value to be 6.0-7.5 by using sodium hydroxide to obtain fermentation liquid containing propionate; 2) carrying out solid-liquid separation on the fermentation liquor, and collecting a liquid phase; 3) concentrating the collected liquid phase by 3-8 times, slowly adding acid under a stirring state, and adjusting the pH value to 2-3.5; 4) distilling the acidized solution under reduced pressure to recover propionic acid; 5) and slowly adding calcium hydroxide into the collected propionic acid, adjusting the pH value to 6.0-8.0, and performing spray drying on the material to obtain a calcium propionate product. The process utilizes the waste liquid to carry out resource regeneration and utilization, obtains the calcium propionate product with higher purity by modes of distillation, calcification and the like, and has high production efficiency, greenness and energy conservation.
Description
Technical Field
The invention belongs to the technical field of biological food preservatives, and particularly relates to a preparation method of fermentation source calcium propionate.
Background
Free propionic acid generated by calcium propionate under acidic condition has wide antibacterial effect on vitamins such as bacteria, mould, yeast and the like, but is harmless to human and livestock and has no toxic or side effect. Therefore, the calcium propionate is a good preservative and fresh-keeping agent in the aspects of food, feed, brewing and the like, and is widely applied in the market. China has a great demand for propionic acid and propionic acid salt as a feed producing country, and shows a trend of increasing year by year.
At present, the main preparation process of calcium propionate mainly comprises chemical synthesis of propionic acid and a calcium source, and although the process has high purity, the production energy consumption is high, and the environment is easily polluted. The preparation process of preparing calcium propionate by a biological fermentation method has been reported, but the technology of producing propionic acid by the existing fermentation method still has some defects, and for example, related documents mention a method for realizing semi-continuous fermentation of propionic acid by using an external plant fiber bed reactor and membrane separation. The production process needs to be filled with nitrogen, so that the control cost is high; the immobilized bagasse material is difficult to be stably recycled; the membrane separation efficiency is low; exogenous addition of fermentation medium with glucose as carbon source is required, resulting in increased costs. For example, CA112176005A, the method produces propionic acid and salt by controlling pH with glucose or sodium hydroxide at different times, and the fermentation product contains a large amount of sodium propionate, so that calcium propionate with high purity cannot be obtained, the fermentation period is long, and the energy consumption is high. In addition, most fermentation methods for preparing calcium propionate adopt the following modes: the calcium source is added directly during the fermentation process. For example, in patent CN103014077, a calcium source is fed during fermentation for 40-60 h, and finally, a solvent is used for crystallization and washing to obtain calcium propionate. In the method, the low-cost calcium carbonate generally has limited solubility in aqueous solution, the fermentation process has higher requirements on equipment, an easily-exploded solvent is adopted in post-treatment, the industrial operation is complicated, and the cost is relatively high.
Disclosure of Invention
In view of the problems in the prior art, the present invention is designed to provide a method for preparing fermentation source calcium propionate. The method adopts the nisin production waste liquid to carry out secondary fermentation to produce propionic acid, is a waste resource recycling method, and is green and energy-saving. After fermentation is finished, the fermentation liquor is acidified and distilled to obtain high-purity propionic acid, and the propionic acid is converted into calcium propionate through calcification, so that the problem that the purity of the product is not high due to entrainment of sodium propionate is solved. Secondly, the post-treatment process is simple, the requirement on equipment is lower, an organic solvent is not involved, the obtained product has high purity and white and bright color, the product quality is greatly improved, and the production cost is reduced.
The invention is realized by the following technical scheme:
the preparation method of the fermentation source calcium propionate is characterized by comprising the following steps:
1) taking nisin fermentation waste liquid as a culture medium, sterilizing at 121 ℃ for 30min, inoculating propionic acid bacteria, fermenting again at 30 ℃ under anaerobic condition, and adding sodium hydroxide to maintain the pH value at 6.0-7.5 to prepare fermentation liquid containing propionate;
2) carrying out solid-liquid separation on the fermentation liquor prepared in the step 1), and collecting a liquid phase;
3) concentrating the liquid phase collected in the step 2) by 3-8 times, slowly adding acid under a stirring state, and adjusting the pH value to 2-3.5 to obtain an acidizing fluid;
4) distilling the acidized fluid under the reduced pressure of-0.075 to-0.095 Mpa to recover propionic acid;
5) slowly adding calcium hydroxide into the propionic acid recovered in the step 4), adjusting the pH value to 6.0-8.0, and performing spray drying on the material to obtain a calcium propionate product.
Further, the inoculation amount of the propionic acid bacteria in the step 1) is 5% -30%, and the propionic acid bacteria are any one of propionibacterium acidovorans and propionibacterium freudenreichii.
Further, the nisin fermentation waste liquid in step 1) is a filtered waste liquid containing 2% -5% lactic acid.
Further, the end time of the secondary fermentation in the step 1) is the end of the consumption of the lactic acid in the nisin fermentation waste liquid.
Further, the solid-liquid separation method in the step 2) adopts any one of plate-and-frame filter pressing, ceramic membrane filtration and hollow fiber membrane filtration.
Further, the acid added in step 3) is any one of hydrochloric acid, sulfuric acid, and nitric acid.
Further, the reduced pressure concentration temperature in the step 4) is 60-100 ℃.
The method of the invention realizes resource recycling by adopting the lactic streptococcal fermentation waste liquid as the culture medium. The method comprises the steps of fermenting the nisin production waste liquid again, culturing thalli by using the residual culture medium components, and converting lactic acid into propionic acid, so that the method is a waste resource recycling method, and is environment-friendly and energy-saving. After fermentation is finished, the fermentation liquor is acidified and distilled to obtain high-purity propionic acid, and then a calcium propionate product with high purity and white and bright color is obtained through a calcification step, so that the product quality and appearance are greatly improved, the production efficiency is improved, and the production cost is reduced.
Drawings
FIG. 1 is a flow chart of a process for preparing calcium propionate.
Detailed Description
The invention is described in further detail below with reference to the drawings and specific examples to understand the technical solution.
The invention relates to a preparation method of fermentation source calcium propionate, which comprises the following steps: 1) Taking nisin fermentation waste liquid as a culture medium, sterilizing at 121 ℃ for 30min, inoculating propionic acid bacteria, fermenting again at 30 ℃ under an anaerobic condition until the lactic acid is consumed, adding sodium hydroxide to maintain the pH value of 6.0-7.5, and preparing fermentation liquid containing propionate, wherein the inoculation amount of the propionic acid bacteria is 5% -30%, the propionic acid bacteria select any one of propionibacterium acidovorans and propionibacterium freudenreichii, and the nisin fermentation waste liquid is filtered waste liquid containing 2% -5% of lactic acid; 2) carrying out solid-liquid separation on the fermentation liquor prepared in the step 1) by adopting plate-and-frame filter pressing, ceramic membrane filtration or hollow fiber membrane filtration, and collecting a liquid phase; 3) Concentrating the liquid phase collected in the step 2) by 3-8 times, and slowly adding any one of hydrochloric acid, sulfuric acid or nitric acid while stirring to adjust the pH to 2-3.5 to obtain an acidizing fluid; 4) distilling the acidized fluid under reduced pressure of-0.075 to-0.095 Mpa at the temperature of 60-100 ℃ to recover propionic acid; 5) slowly adding calcium hydroxide into the propionic acid recovered in the step 4), adjusting the pH value to 6.0-8.0, and performing spray drying on the material to obtain a calcium propionate product.
Example 1
Taking the waste liquid obtained after separation of nisin bacterial liquid as a culture medium, measuring the lactic acid in the culture medium to be 40g/L, sterilizing at 121 ℃ for 30min, inoculating 20% propionibacterium freudenreichii seed liquid, performing anaerobic fermentation at 30 ℃, maintaining the pH value to be 6.8-7.2 by 30% sodium hydroxide, sampling in the process, analyzing the content of the lactic acid until the lactic acid is consumed, and finishing the fermentation. Filtering the fermentation liquor containing propionate with ceramic membrane to remove mycelium, and collecting clear liquid containing 25g/L sodium propionate. Concentrating 1000ml of collected liquid phase at 70 ℃ under reduced pressure for 5 times, slowly adding 30ml of 50% (v: v) sulfuric acid under stirring to adjust the pH value to 3.07, distilling the acidified liquid at 70 ℃ under reduced pressure of-0.09 Mpa to recover 203ml of propionic acid, slowly adding 15g of calcium hydroxide under stirring to adjust the pH value to 7.0, and then carrying out spray drying to obtain a white powdery calcium propionate product with the content of 62.5% and the post-treatment yield of 83%.
Example 2
Taking the waste liquid obtained after separation of nisin bacterial liquid as a culture medium, measuring the lactic acid in the culture medium to be 40g/L, sterilizing at 121 ℃ for 30min, inoculating 30% propionibacterium freudenreichii seed liquid, performing anaerobic fermentation at 30 ℃, maintaining the pH value to be 6.8-7.2 by 30% sodium hydroxide, sampling in the process, analyzing the content of the lactic acid until the lactic acid is consumed, and finishing the fermentation. Filtering the fermentation liquor containing propionate with ceramic membrane to remove mycelium, and collecting clear liquid containing 25g/L sodium propionate. Concentrating 1000ml of collected liquid phase at 70 ℃ under reduced pressure for 5 times, slowly adding 51ml of concentrated hydrochloric acid under the stirring state, adjusting the pH value to 3.11, distilling the acidified liquid at 70 ℃ under reduced pressure of-0.09 Mpa to recover 230ml of propionic acid, slowly adding 15.6g of calcium hydroxide under the stirring state, adjusting the pH value to 7.05, and then carrying out spray drying to obtain a white powdery calcium propionate product with the content of 68.68% and the post-treatment yield of 87.62%.
Example 3
Taking the waste liquid obtained after the separation of the nisin bacterial liquid as a culture medium, measuring the lactic acid in the culture medium to be 41.5g/L, sterilizing at 121 ℃ for 30min, inoculating 30% of acid-producing propionibacterium acidi seed liquid, performing anaerobic fermentation at 30 ℃, maintaining the pH value to be 6.8-7.2 by 30% of sodium hydroxide, sampling in the process, analyzing the content of the lactic acid until the lactic acid is consumed, and finishing the fermentation. Filtering the fermentation liquor containing propionate with ceramic membrane to remove mycelium, and collecting clear liquid containing 27.8g/L sodium propionate. Collecting 1000ml of liquid phase, concentrating under reduced pressure at 70 ℃ for 5 times, slowly adding 48ml of concentrated hydrochloric acid under stirring, adjusting the pH value to 2.98, distilling the acidified liquid under reduced pressure of 70 ℃ to 0.09Mpa to recover 225ml of propionic acid, slowly adding 16g of calcium hydroxide under stirring, adjusting the pH value to 7.04, and performing spray drying to obtain a white powdery calcium propionate product with the content of 68% and the post-treatment yield of 85.03%.
Claims (7)
1. A preparation method of fermentation source calcium propionate is characterized by comprising the following steps:
1) taking nisin fermentation waste liquid as a culture medium, sterilizing at 121 ℃ for 30min, inoculating propionic acid bacteria, fermenting again at 30 ℃ under anaerobic condition, and adding sodium hydroxide to maintain the pH value at 6.0-7.5 to prepare fermentation liquid containing propionate;
2) carrying out solid-liquid separation on the fermentation liquor prepared in the step 1), and collecting a liquid phase;
3) concentrating the liquid phase collected in the step 2) by 3-8 times, slowly adding acid under a stirring state, and adjusting the pH value to 2-3.5 to obtain an acidizing fluid;
4) distilling the acidized fluid under the reduced pressure of-0.075 to-0.095 Mpa to recover propionic acid;
5) slowly adding calcium hydroxide into the propionic acid recovered in the step 4), adjusting the pH value to 6.0-8.0, and performing spray drying on the material to obtain a calcium propionate product.
2. The method for preparing fermentation source calcium propionate according to claim 1, wherein the inoculation amount of the propionic acid bacteria in step 1) is 5% -30%, and the propionic acid bacteria is any one of propionibacterium acidovorans and propionibacterium freudenreichii.
3. The method for preparing fermentation source calcium propionate according to claim 1, wherein the nisin fermentation waste liquid in step 1) is a filtered waste liquid containing 2% -5% lactic acid.
4. The method for preparing fermentation source calcium propionate according to claim 1, wherein the end time of the secondary fermentation in step 1) is the end of the consumption of lactic acid in the waste fermentation liquid of nisin.
5. The method for preparing fermentation source calcium propionate according to claim 1, wherein the solid-liquid separation method in step 2) is any one of plate-and-frame filter pressing, ceramic membrane filtration and hollow fiber membrane filtration.
6. The method for preparing fermentation source calcium propionate according to claim 1, wherein the acid added in step 3) is any one of hydrochloric acid, sulfuric acid and nitric acid.
7. The method for preparing fermentation source calcium propionate according to claim 1, wherein the concentration under reduced pressure in step 4) is at a temperature of 60-100 ℃.
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CN103014077A (en) * | 2012-12-27 | 2013-04-03 | 天津科百生物科技研发有限公司 | Novel process for producing calcium propionate by fermentation method |
CN110607329A (en) * | 2019-10-25 | 2019-12-24 | 浙江圣达生物研究院有限公司 | Method for producing propionic acid by fermentation |
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Patent Citations (4)
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CN1458138A (en) * | 2003-05-15 | 2003-11-26 | 河北科技大学 | Acidifying, distilling and extracting method for natural propionic acid and acetic acid of propionic bacteria fermentation liquid |
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