CN110857446A - Production process of high-purity lactic acid - Google Patents
Production process of high-purity lactic acid Download PDFInfo
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- CN110857446A CN110857446A CN201810969198.2A CN201810969198A CN110857446A CN 110857446 A CN110857446 A CN 110857446A CN 201810969198 A CN201810969198 A CN 201810969198A CN 110857446 A CN110857446 A CN 110857446A
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000004310 lactic acid Substances 0.000 title claims abstract description 51
- 235000014655 lactic acid Nutrition 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 238000000855 fermentation Methods 0.000 claims abstract description 62
- 230000004151 fermentation Effects 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 240000005384 Rhizopus oryzae Species 0.000 claims abstract description 29
- 235000013752 Rhizopus oryzae Nutrition 0.000 claims abstract description 29
- 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 claims abstract description 16
- 239000008103 glucose Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 230000000694 effects Effects 0.000 claims abstract description 10
- 238000003860 storage Methods 0.000 claims description 27
- 238000005086 pumping Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000005342 ion exchange Methods 0.000 claims description 16
- 238000001704 evaporation Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000011575 calcium Substances 0.000 claims description 12
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims description 12
- 239000001527 calcium lactate Substances 0.000 claims description 12
- 229960002401 calcium lactate Drugs 0.000 claims description 12
- 235000011086 calcium lactate Nutrition 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 230000001954 sterilising effect Effects 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229960005069 calcium Drugs 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 6
- 238000009924 canning Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000001728 nano-filtration Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000008394 flocculating agent Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 235000000346 sugar Nutrition 0.000 claims description 5
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 4
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 3
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 3
- 238000005349 anion exchange Methods 0.000 claims description 3
- 238000005341 cation exchange Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000003311 flocculating effect Effects 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 3
- 239000012047 saturated solution Substances 0.000 claims description 3
- 238000005056 compaction Methods 0.000 claims description 2
- 239000012527 feed solution Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000008188 pellet Substances 0.000 abstract description 6
- 238000004220 aggregation Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- 238000007711 solidification Methods 0.000 abstract description 2
- 241000894006 Bacteria Species 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000002255 enzymatic effect Effects 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000747 poly(lactic acid) Polymers 0.000 description 2
- 239000004626 polylactic acid Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 1
- GAWAYYRQGQZKCR-UHFFFAOYSA-N 2-chloropropionic acid Chemical compound CC(Cl)C(O)=O GAWAYYRQGQZKCR-UHFFFAOYSA-N 0.000 description 1
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 description 1
- 208000010444 Acidosis Diseases 0.000 description 1
- 241001550224 Apha Species 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 208000002682 Hyperkalemia Diseases 0.000 description 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 1
- 241000235342 Saccharomycetes Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000007950 acidosis Effects 0.000 description 1
- 208000026545 acidosis disease Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229920000704 biodegradable plastic Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 229940001447 lactate Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 229940107700 pyruvic acid Drugs 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 239000001540 sodium lactate Substances 0.000 description 1
- 229940005581 sodium lactate Drugs 0.000 description 1
- 235000011088 sodium lactate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance 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
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
- C12P7/56—Lactic acid
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- 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 high-purity lactic acid preparation process, which adopts glucose as a raw material and rhizopus oryzae as a fermentation strain, wherein in the strain preparation process, hyphae of the rhizopus oryzae are subjected to self-aggregation to form rhizopus oryzae pellets to achieve the self-solidification effect, the large-area aggregation of the free hyphae is avoided to prevent the mass transfer of materials, the strain is easy to separate from a feed liquid after fermentation, and the separated strain can be recycled.
Description
Technical Field
The invention relates to the technical field of fermentation engineering, in particular to a production process of high-purity lactic acid.
Background
Lactic acid has many uses in industry, food, medicine, and the like, and is widely used as a preservative, an acidulant, and a reducing agent. In the production process of cans, sauces and beverages, lactic acid can replace preservatives such as benzoic acid, potassium sorbate and the like which have side effects on human bodies, and can be used as a sour agent of the foods; in the production process of the beer, the pH value can be adjusted by using lactic acid, so that the saccharification of raw materials can be promoted, and the growth of mixed bacteria can be inhibited; lactic acid has many important applications in medical applications, both as a disinfectant and as a carrier; the solution prepared from sodium lactate can be used for treating acidosis and hyperkalemia; the lactate substances can be used as a solvent of the medicine, increase the absorption of the medicine by human body, reduce side effects, and can also be prepared into a lubricant of a tablet, wherein the lubricant is prepared from polylactic acid and is widely applied clinically, such as a slow release capsule preparation, a biodegradable surgical suture, a biological implantation tablet and the like; in the chemical industry, lactic acid is the main raw material of biodegradable plastic polylactic acid; the lactic acid can also be used in the leather manufacturing industry to ensure that the leather is soft and fine and the fiber is glossy; lactic acid can also be used as a synthetic resin coating, an adhesive, a perfume and a cleaning agent for petroleum pipelines.
In the prior art, chemical synthesis, enzymatic synthesis and fermentation methods are mostly adopted for producing lactic acid, wherein the chemical synthesis method has the defects that the production raw materials are toxic and the lactic acid with single optical rotation property cannot be produced, and toxic chemical substances in the lactic acid produced by the chemical synthesis method are removed when the lactic acid is used as a food additive, so that the treatment difficulty is increased, and the production process is complex; the enzymatic synthesis method is only a 1, 2-chloropropionic acid enzymatic method and a pyruvic acid enzymatic conversion method, but both methods have the defect of complex production process, are not suitable for modern industrial production, and are mainly used for laboratory research and the like; the fermentation method for producing lactic acid has the advantages of simple and convenient process, mild production conditions, high photochemical purity of products and the like, so the method is widely applied to industrial production.
The fermentation method mainly comprises the steps of fermenting saccharides by adopting lactic acid bacteria, adding calcium carbonate for neutralization, filtering, carrying out acidolysis and purifying to obtain pure lactic acid. However, the lactic acid produced by the fermentation method in the prior art has many defects of low raw material conversion rate, long fermentation period, low product purity and the like, so that the raw material utilization rate, the production efficiency and the finished product quality are low, the lactic acid bacteria cannot be recycled after being fermented once, and the industrial production is not facilitated, so that how to provide a lactic acid production process with high raw material conversion rate, short fermentation period, recyclable bacteria and high product purity is an urgent problem to be solved by technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides a method for producing lactic acid by fermentation of glucose, wherein raw materials in a fermentation liquid are fully utilized, a fermentation period is shortened by controlling fermentation conditions, fermentation efficiency is improved, a product has higher purity by multiple post-purification processes, and strains can be repeatedly utilized, thereby increasing economic benefits.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of high-purity lactic acid comprises the following steps:
(1) preparing raw materials: injecting a proper amount of water into the seasoning tank, heating the water to 50 ℃, opening the stirrer, pouring glucose powder, dissolving and stirring uniformly, adjusting the pH value to be between 5.5 and 6.0, and transferring the solution into a sugar solution storage tank for later use;
(2) heating and sterilizing: sterilizing material conveying equipment and fermentation equipment by adopting high-temperature steam, starting a material transferring pump after the material conveying equipment and the fermentation equipment are sterilized, enabling the material to enter a fermentation tank through an injection pump, simultaneously introducing the high-temperature steam into the injection pump, and heating and sterilizing the material by the high-temperature steam;
(3) fermentation: cooling the sterilized equipment and materials in the step (2) to 45-48 ℃, inoculating the strain into a fermentation tank, starting fermentation, keeping the temperature in the fermentation tank at 45-50 ℃ and the pressure at 0.4-0.8 Mpa, and adding Ca (OH)2The pH value of the feed liquid is maintained to be 5.5-6.0 by the saturated solution, the glucose content in the feed liquid is detected, and when the glucose content is 0, the fermentation is finished;
(4) and (3) filtering and flocculating: filtering to remove strains after the fermentation in the step (3), recovering the strains for later use, adjusting the pH value of the filtrate, and adding a flocculating agent to flocculate impurities;
(5) plate and frame filter pressing: transferring the flocculated material obtained in the step (4) into a fermentation liquor storage tank, pumping the material into a plate-and-frame filter press by using a pump, removing flocculation under the feeding pressure of 0.4-0.5Mpa and the pressing pressure of 15-20Mpa, and transferring the plate-and-frame filtrate, namely calcium lactate, into a fermentation clear liquid storage tank;
(6) calcium lactate evaporation and concentration: pumping the calcium lactate obtained in the step (5) into an evaporator, starting a water ring vacuum pump for evaporation and concentration, and discharging the material into a calcium concentrated solution storage tank;
(7) acid hydrolysis: pumping the calcium lactate concentrated solution obtained in the step (6) into an acidolysis tank, feeding at the temperature of 75-80 ℃, and then adding sulfuric acid into the acidolysis tank for acidolysis;
(8) and (3) filtering: pumping the acidolysis solution after the acidolysis end point in the step (7) into a belt filter by using a vacuum pump, and filtering filtrate after calcium sulfate;
(9) and (3) decoloring: pumping the filtrate obtained in the step (8) into a decoloring tank, heating to 70-72 ℃, and adding activated carbon to decolor;
(10) plate and frame filter pressing: performing plate-and-frame filter pressing on the material decolorized in the step (9), filtering out active carbon in the material, and feeding filtrate into a decolorized clear liquid storage tank;
(11) ion exchange: sequentially passing the decolorized clear liquid obtained in the step (10) through a carbon column, a cation exchange column and an anion exchange column to remove impurities, and then entering an ion exchange liquid storage tank;
(12) MVR evaporation and concentration: starting a vacuum pump and a steam compressor, starting steam, heating the system, evaporating and concentrating the ion exchange liquid obtained in the step (11), and pumping the concentrated liquid into a storage tank before the membrane;
(13) and (3) nanofiltration membrane filtration: adjusting the pressure difference between the feeding and the discharging to be less than or equal to 0.5Mpa, leading the concentrated solution obtained in the step (12) to pass through a nanofiltration membrane, filtering impurities, and leading the filtrate to enter a membrane post-tank;
(14) concentrating by a plate evaporator: pumping the filtrate obtained in the step (13) into a plate evaporator, wherein the feeding flow rate is 5.2-6.0m3Heating by steam, controlling the air inlet pressure of a heat pump to be 0.35-0.4Mpa, controlling the discharge density to be 1.14-1.20kg/L, controlling the discharge concentration to reach more than 80%, and pumping into a finished product storage tank;
(15) blending and canning: and (5) detecting the material concentration in the finished product storage tank in the step (14), pumping the finished product into a blending tank according to the requirement, blending and then canning.
By adopting the scheme, the invention provides the lactic acid preparation process with higher raw material utilization rate, and the product lactic acid has higher purity through the multi-stage subsequent purification process, and the process is simple, convenient and controllable.
Preferably, the adding amount of the glucose in the step (1) is adjusted according to the concentration required by production.
Preferably, the fermentation strain in the step (3) is fermented by rhizopus oryzae, the rhizopus oryzae is granular rhizopus oryzae which is cultured and self-flocculated by hypha, the volume of the inoculated mold liquid is 10-15% of the total volume of the feed liquid in the fermentation tank, and the added yeast powder is 0.15-0.20% of the rhizopus oryzae.
The beneficial effects of the preferred technical scheme are as follows: the rhizopus oryzae needs to be immobilized to avoid the aggregation of a large amount of free hyphae to block the mass transfer of materials when the rhizopus oryzae is fermented to produce lactic acid, the rhizopus oryzae aggregated into small particles plays a self-curing role, the production efficiency of the lactic acid is ensured, the rhizopus oryzae particle strains are easy to separate from products and can be recycled, and the saccharomycetes and the rhizopus oryzae are added to jointly act, so that the fermentation speed is increased, the fermentation period is shortened, and the economic benefit is increased.
Preferably, the flocculant added in the step (4) is a chitosan flocculant, the pH of the adjusted feed liquid is 3.9-4.1, and the concentration of the flocculant is 50mg/m3The amount of the flocculant added was 50mg/m3And adding a flocculating agent and stirring for 4-6 min.
Preferably, the evaporator in the step (6) is a three-effect evaporator, the concentration process comprises feeding into the three-effect evaporator, then entering into the first effect, simultaneously starting steam to boil the material, then entering into the second effect, keeping the temperature above 75 ℃, and reaching the concentration end point when the concentration of the second-effect calcium reaches 20%.
The beneficial effects of the preferred technical scheme are as follows: the balance of the temperature, the concentration and the viscosity of the feed liquid is facilitated, the scaling of an evaporator and the browning of the feed liquid are prevented, and the evaporation efficiency is improved.
Preferably, Ca is added in the step (7) when the pH value reaches 2-2.52﹢The concentration of 0.25-0.5% is the acid hydrolysis end point.
Preferably, the color of the feed liquid is decolorized in the step (9) until the color of the feed liquid is less than Y-3.
Preferably, the ion exchange flow of the feed liquid in the step (11) is 7-12 m3/h，Fe3﹢≤10PPm,Cl﹣≤20PPm，SO4 2﹣The color is less than or equal to 50PPm, and the color is less than or equal to 50APHA, namely the ion exchange is qualified.
Preferably, the discharge density of MVR evaporation concentration in the step (12) is 1.116-1.118 kg/L.
Preferably, the water for blending the materials in the step (15) is softened tap water, and the conductivity of the softened tap water is less than or equal to 20 mu s/cm.
According to the technical scheme, compared with the prior art, the invention discloses a high-purity lactic acid preparation process, glucose is used as a raw material, rhizopus oryzae is used as a fermentation strain, during the preparation process, the rhizopus oryzae mycelia are self-agglomerated to form rhizopus oryzae pellets to achieve the self-solidification effect, the situation that the mass transfer of materials is hindered by large-area agglomeration of free mycelia is avoided, the strain is easy to separate from a feed liquid after fermentation, the separated strain can be recycled, and importantly, lactic acid products fermented by the rhizopus oryzae have high optical purity and high raw material utilization rate, and a plurality of subsequent purification treatment steps are combined to ensure that the lactic acid products have high purity.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
The high-purity lactic acid is produced by adopting the following process steps:
(1) preparing raw materials: injecting a proper amount of water into the seasoning tank, heating the water to 50 ℃, opening the stirrer, pouring a proper amount of glucose powder according to the required concentration, dissolving and uniformly stirring, adjusting the pH value to be between 5.5 and 6.0, and transferring the mixture into a sugar liquid storage tank for later use;
(2) heating and sterilizing: sterilizing material conveying equipment and fermentation equipment by adopting high-temperature steam, starting a material transferring pump after the material conveying equipment and the fermentation equipment are sterilized, enabling the material to enter a fermentation tank through an injection pump, simultaneously introducing the high-temperature steam into the injection pump, and heating and sterilizing the material by the high-temperature steam;
(3) fermentation: cooling the sterilized equipment and materials in the step (2) to 45-48 ℃, inoculating granular rhizopus oryzae liquid accounting for 10% -15% of the total volume of the materials in the fermentation tank into the fermentation tank, adding a proper amount of yeast to start fermentation, keeping the temperature in the fermentation tank at 45-50 ℃ and the pressure at 0.4-0.8 Mpa, and adding Ca (OH)2The pH of the feed liquid is maintained to be 5.5-6.0 by the saturated solution, the glucose content in the feed liquid is detected, and when the glucose content is 0, the fermentation is finished;
(4) and (3) filtering and flocculating: filtering to remove strains after the fermentation in the step (3), recovering the strains for later use, adjusting the pH value of the filtrate to 3.9-4.1, and adjusting the pH value to 50mg/m3Is added in an amount of 50mg/m3Stirring the chitosan flocculating agent for 4-6 min to flocculate impurities;
(5) plate and frame filter pressing: transferring the flocculated material obtained in the step (4) into a fermentation liquor storage tank, pumping the material into a plate and frame filter press by using a pump, removing flocculation, wherein the feeding pressure is 0.4-0.5Mpa, the compaction pressure is 15-20Mpa, and the plate and frame filtrate is calcium lactate and is transferred into a fermentation clear liquid storage tank;
(6) calcium lactate evaporation and concentration: pumping the calcium lactate obtained in the step (5) into a triple-effect evaporator, starting a water ring vacuum pump, feeding the triple-effect material into a first effect, starting steam to boil the material, feeding the triple-effect material into a second effect, keeping the temperature above 75 ℃, performing evaporation concentration when the concentration of the double-effect calcium reaches 20%, and discharging the triple-effect material into a calcium concentrated solution storage tank;
(7) acid hydrolysis: pumping the calcium lactate concentrated solution obtained in the step (6) into an acidolysis tank, feeding at the temperature of 75-80 ℃, adding sulfuric acid into the acidolysis tank for acidolysis, and adding Ca when the pH reaches 2-2.52﹢The concentration of 0.25-0.5 percent is the acidolysis end point;
(8) and (3) filtering: pumping the acidolysis solution after the acidolysis end point in the step (7) into a belt filter by using a vacuum pump, and filtering filtrate after calcium sulfate;
(9) and (3) decoloring: pumping the filtrate obtained in the step (8) into a decoloring tank, heating to 70-72 ℃, adding activated carbon to decolor until the chroma of the feed liquid is less than Y-3;
(10) plate and frame filter pressing: performing plate-and-frame filter pressing on the material decolorized in the step (9), filtering out active carbon in the material, and feeding filtrate into a decolorized clear liquid storage tank;
(11) ion exchange: removing impurities in the decolorized clear liquid obtained in the step (10) through a carbon column, a cation exchange column and an anion exchange column in sequence, wherein the ion exchange flow of the feed liquid is 7-12 m3/h，Fe3﹢≤10PPm, Cl﹣≤20PPm，SO4 2﹣The ion exchange is qualified when the chromaticity is less than or equal to 50PPm and the APHA is less than or equal to 50, and then the ion exchange enters an ion exchange liquid storage tank;
(12) MVR evaporation and concentration: starting a vacuum pump and a steam compressor, starting steam, heating a system, evaporating and concentrating the ion exchange liquid obtained in the step (11) until the discharge density is 1.116-1.118kg/L, and pumping the concentrated liquid into a storage tank before the membrane;
(13) and (3) nanofiltration membrane filtration: adjusting the pressure difference between the feeding and the discharging to be less than or equal to 0.5Mpa, leading the concentrated solution obtained in the step (12) to pass through a nanofiltration membrane, filtering impurities, and leading the filtrate to enter a membrane post-tank;
(14) concentrating by a plate evaporator: pumping the filtrate obtained in the step (13) into a plate evaporator, wherein the feeding flow rate is 5.2-6.0m3Heating by steam, controlling the air inlet pressure of a heat pump to be 0.35-0.4Mpa, controlling the discharge density to be 1.14-1.20kg/L, controlling the discharge concentration to reach more than 80%, and pumping into a finished product storage tank;
(15) blending and canning: and (5) detecting the material concentration in the finished product storage tank in the step (14), pumping the finished product into a blending tank according to the requirement, blending by using softened tap water with the conductivity of less than or equal to 20 mu s/cm, and canning.
Comparative example 1
The lactic acid is produced by adopting a common lactic acid bacteria fermentation process.
Example 2
Parameters in the lactic acid production process and quality testing of lactic acid products:
in the production process for preparing the lactic acid by adopting the technical scheme of the invention, the fermentation time is 17 hours; the purity of the product lactic acid was 99.8% and the residual total sugars was 0.15%.
The fermentation time required for lactic acid preparation using the technical scheme of comparative example 1 was 28 hours; the purity of the product lactic acid was 97.5% and the residual total sugars 0.4%.
The granular rhizopus oryzae is adopted for fermentation, the filtered granular rhizopus oryzae can be recycled and has higher performance, and the glucose conversion rate of the rhizopus oryzae recycled for multiple times is as follows by adopting the technical scheme of the invention:
the results show that the rhizopus oryzae adopted by the invention has the characteristic of repeated utilization, the conversion rate of glucose can reach 71% in the 16 th utilization, and the conversion rate is rapidly reduced in the 17 th fermentation, and the reason is that the rhizopus oryzae pellets are gradually increased, broken and inactivated in the utilization process, so that the rhizopus oryzae pellets are adopted for fermentation to produce lactic acid, and the rhizopus oryzae pellets can be repeatedly utilized for 16 times, so that the rhizopus oryzae pellets have higher economic benefit.
In contrast, in comparative example 1, lactic acid bacteria were removed together with flocs in the flocculation stage, and could not be reused.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A production process of high-purity lactic acid is characterized by comprising the following steps:
(1) preparing raw materials: injecting a proper amount of water into the seasoning tank, heating the water to 50 ℃, opening the stirrer, pouring glucose powder, dissolving and stirring uniformly, adjusting the pH value to be between 5.5 and 6.0, and transferring the solution into a sugar solution storage tank for later use;
(2) heating and sterilizing: sterilizing material conveying equipment and fermentation equipment by adopting high-temperature steam, starting a material transferring pump after the material conveying equipment and the fermentation equipment are sterilized, enabling the material to enter a fermentation tank through an injection pump, simultaneously introducing the high-temperature steam into the injection pump, and heating and sterilizing the material by the high-temperature steam;
(3) fermentation: cooling the sterilized equipment and materials in the step (2) to 45-48 ℃, inoculating the strain into a fermentation tank, starting fermentation, keeping the temperature in the fermentation tank at 45-50 ℃ and the pressure at 0.4-0.8 Mpa, and adding Ca (OH)2The pH of the feed liquid is maintained to be 5.5-6.0 by the saturated solution, the glucose content in the feed liquid is detected, and when the glucose content is 0, the fermentation is finished;
(4) and (3) filtering and flocculating: filtering to remove strains after the fermentation in the step (3), recovering the strains for later use, adjusting the pH value of the filtrate, and adding a flocculating agent to flocculate impurities;
(5) plate and frame filter pressing: transferring the flocculated material obtained in the step (4) into a fermentation liquor storage tank, feeding the material into a plate-and-frame filter press by using a pump, removing flocculation residues under the feeding pressure of 0.4-0.5Mpa and the compaction pressure of 15-20Mpa, and transferring the plate-and-frame filtrate, namely calcium lactate, into a fermentation clear liquid storage tank;
(6) calcium lactate evaporation and concentration: pumping the calcium lactate obtained in the step (5) into an evaporator, starting a water ring vacuum pump for evaporation and concentration, and discharging the material into a calcium concentrated solution storage tank;
(7) acid hydrolysis: pumping the calcium lactate concentrated solution obtained in the step (6) into an acidolysis tank, feeding at the temperature of 75-80 ℃, and then adding sulfuric acid into the acidolysis tank for acidolysis;
(8) and (3) filtering: pumping the acidolysis solution after the acidolysis end point in the step (7) into a belt filter by using a vacuum pump, and filtering filtrate after calcium sulfate;
(9) and (3) decoloring: pumping the filtrate obtained in the step (8) into a decoloring tank, heating to 70-72 ℃, and adding activated carbon to decolor;
(10) plate and frame filter pressing: performing plate-and-frame filter pressing on the material decolorized in the step (9), filtering out active carbon in the material, and feeding filtrate into a decolorized clear liquid storage tank;
(11) ion exchange: sequentially passing the decolorized clear liquid obtained in the step (10) through a carbon column, a cation exchange column and an anion exchange column to remove impurities, and then entering an ion exchange liquid storage tank;
(12) MVR evaporation and concentration: starting a vacuum pump and a steam compressor, starting steam, heating the system, evaporating and concentrating the ion exchange liquid obtained in the step (11), and pumping the concentrated liquid into a storage tank before the membrane;
(13) and (3) nanofiltration membrane filtration: adjusting the pressure difference between the feeding and the discharging to be less than or equal to 0.5Mpa, leading the concentrated solution obtained in the step (12) to pass through a nanofiltration membrane, filtering impurities, and leading the filtrate to enter a membrane post-tank;
(14) concentrating by a plate evaporator: pumping the filtrate obtained in the step (13) into a plate evaporator, wherein the feeding flow rate is 5.2-6.0m3Heating by steam, controlling the air inlet pressure of a heat pump to be 0.35-0.4Mpa, controlling the discharge density to be 1.14-1.20kg/L, controlling the discharge concentration to reach more than 80%, and pumping into a finished product storage tank;
(15) blending and canning: and (5) detecting the material concentration in the finished product storage tank in the step (14), pumping the finished product into a blending tank according to the requirement, blending and then canning.
2. The process for producing high-purity lactic acid according to claim 1, wherein the amount of glucose added in step (1) is adjusted according to the concentration required for production.
3. The process for producing high-purity lactic acid according to claim 1, wherein the fermentation strain in the step (3) is fermented by rhizopus oryzae, the rhizopus oryzae is granular rhizopus oryzae which is cultured and self-flocculated by hyphae, the volume of the inoculated mold solution is 10-15% of the total volume of the feed solution in the fermentation tank, and the ratio of the added yeast powder to the rhizopus oryzae is 0.15-0.2%.
4. The process for producing high-purity lactic acid according to claim 1, wherein the flocculant added in the step (4) is a chitosan flocculant, the pH of the adjusted feed liquid is 3.9-4.1, and the concentration of the flocculant is 50mg/m3The amount of the flocculant added was 50mg/m3And adding a flocculating agent and stirring for 4-6 min.
5. The process for producing high-purity lactic acid according to claim 1, wherein the evaporator in the step (6) is a triple-effect evaporator, the concentration process comprises feeding the triple-effect evaporator, then feeding the triple-effect evaporator into a first effect, starting steam to boil the materials, then feeding the triple-effect evaporator into a second effect, keeping the temperature above 75 ℃, and reaching the concentration end point when the concentration of the double-effect calcium reaches 20%.
6. The process for producing high-purity lactic acid according to claim 1, wherein Ca is decomposed when pH is 2 to 2.5 in the step (7)2﹢The concentration of 0.25-0.5% is the acidolysis end point.
7. The process for producing high-purity lactic acid according to claim 1, wherein the color of the feed liquid in the step (9) is reduced to a color of less than Y-3.
8. The production process of high-purity lactic acid according to claim 1, wherein the ion exchange flow rate of the feed liquid in the step (11) is 7-12 m3/h，Fe3﹢≤10PPm,Cl﹣≤20PPm，SO4 2﹣The color is less than or equal to 50PPm, and the color is less than or equal to 50APHA, namely the ion exchange is qualified.
9. The process for producing high-purity lactic acid according to claim 1, wherein the MVR evaporation concentration in the step (12) has a discharge density of 1.116-1.118 kg/L.
10. The process for producing high-purity lactic acid according to claim 1, wherein the water used for blending the materials in the step (15) is softened tap water, and the conductivity of the water is less than or equal to 20 μ s/cm.
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