CN115259209A - Method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as raw material - Google Patents
Method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as raw material Download PDFInfo
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- CN115259209A CN115259209A CN202211021660.9A CN202211021660A CN115259209A CN 115259209 A CN115259209 A CN 115259209A CN 202211021660 A CN202211021660 A CN 202211021660A CN 115259209 A CN115259209 A CN 115259209A
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- 229960001763 zinc sulfate Drugs 0.000 title claims abstract description 66
- 229910000368 zinc sulfate Inorganic materials 0.000 title claims abstract description 66
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000002994 raw material Substances 0.000 title claims abstract description 18
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 title claims abstract 35
- 238000003756 stirring Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 21
- 238000000855 fermentation Methods 0.000 claims description 16
- 230000004151 fermentation Effects 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 244000005700 microbiome Species 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 229920005615 natural polymer Polymers 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 7
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000000813 microbial effect Effects 0.000 claims description 6
- 230000001954 sterilising effect Effects 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- RMBLTWUTZAFABA-XVSDJDOKSA-N (5z,8z,11z,14z)-icosa-5,8,11,14-tetraenoic acid;sodium Chemical compound [Na].CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O RMBLTWUTZAFABA-XVSDJDOKSA-N 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 4
- 241001225321 Aspergillus fumigatus Species 0.000 claims description 4
- 244000063299 Bacillus subtilis Species 0.000 claims description 4
- 235000014469 Bacillus subtilis Nutrition 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000161 Locust bean gum Polymers 0.000 claims description 4
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 4
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 4
- 241000187561 Rhodococcus erythropolis Species 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 229940091771 aspergillus fumigatus Drugs 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- QKIUAMUSENSFQQ-UHFFFAOYSA-N dimethylazanide Chemical compound C[N-]C QKIUAMUSENSFQQ-UHFFFAOYSA-N 0.000 claims description 4
- CJMZLCRLBNZJQR-UHFFFAOYSA-N ethyl 2-amino-4-(4-fluorophenyl)thiophene-3-carboxylate Chemical compound CCOC(=O)C1=C(N)SC=C1C1=CC=C(F)C=C1 CJMZLCRLBNZJQR-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000011081 inoculation Methods 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 235000010420 locust bean gum Nutrition 0.000 claims description 4
- 239000000711 locust bean gum Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 235000013527 bean curd Nutrition 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- 238000004659 sterilization and disinfection Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 2
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 description 33
- 229910052793 cadmium Inorganic materials 0.000 description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 206010048259 Zinc deficiency Diseases 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- -1 astringent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002895 emetic Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/06—Sulfates
-
- 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
- C12N1/14—Fungi; Culture media therefor
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
- C12R2001/00—Microorganisms ; Processes using microorganisms
- C12R2001/01—Bacteria or Actinomycetales ; using bacteria or Actinomycetales
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
- C12R2001/00—Microorganisms ; Processes using microorganisms
- C12R2001/01—Bacteria or Actinomycetales ; using bacteria or Actinomycetales
- C12R2001/07—Bacillus
- C12R2001/125—Bacillus subtilis ; Hay bacillus; Grass bacillus
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
- C12R2001/00—Microorganisms ; Processes using microorganisms
- C12R2001/645—Fungi ; Processes using fungi
- C12R2001/66—Aspergillus
- C12R2001/68—Aspergillus fumigatus
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Genetics & Genomics (AREA)
- Biotechnology (AREA)
- Zoology (AREA)
- Wood Science & Technology (AREA)
- General Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Microbiology (AREA)
- Virology (AREA)
- Tropical Medicine & Parasitology (AREA)
- Biochemistry (AREA)
- General Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Mycology (AREA)
- Botany (AREA)
- Inorganic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material, and relates to the technical field of chemical industry. The method for producing the food-grade zinc sulfate by using the industrial-grade zinc sulfate as the raw material comprises the following preparation steps of adding the industrial zinc sulfate into distilled water, stirring and mixing, then decoloring, adding the composite extracting agent and the oxidant, standing and layering, then adding the composite bioflocculant, stirring, heating in a water bath, then putting into a vacuum environment for concentrating, finally cooling and crystallizing, and centrifugally drying to obtain the food-grade zinc sulfate. Food-grade zinc sulfate is produced by taking industrial-grade zinc sulfate as a raw material, so that the production cost of the food-grade zinc sulfate is greatly reduced, the preparation time is faster, the yield is higher, the composite bioflocculant prepared is added in the process of the food-grade zinc sulfate, the edible safety is higher after the product is produced, the pollution is less, and the environment is protected.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material.
Background
Zinc sulfate is mainly used as raw material for preparing lithopone, lithopone and other zinc compounds, and also as nutritional material for animals in case of zinc deficiency, feed additive for animal husbandry, zinc fertilizer (trace element fertilizer) for crops, important material for artificial fiber, electrolyte for electrolytic production of metal zinc, mordant in textile industry, medicinal emetic agent, astringent, fungicide, wood and leather preservative, etc.
With the rapid development of production and living, the demand of food-grade zinc sulfate increases day by day, but at present, the food-grade zinc sulfate is mainly prepared by taking sphalerite as a raw material through a series of processing operations, a large amount of harmful gas is generated in the processing process, the raw material cost is high, the utilization rate is low, and the finished product is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material, and solves the problems of high preparation cost, low utilization rate of the raw material and great environmental pollution in the production process of the food-grade zinc sulfate.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material comprises the following preparation steps:
adding distilled water, stirring and fully mixing and dissolving to obtain a mixed solution;
s2: adding a decoloring agent into the mixed liquid obtained in the step S1 for decoloring, and then filtering to obtain a filtrate;
s3: adding a composite extracting agent and an oxidant into the filtrate obtained in the step S2, heating by adopting a water bath method, mixing, stirring and oscillating, standing for layering, and taking the upper-layer solution to obtain a layering solution for later use;
s4: taking a certain amount of bean curd wastewater, adjusting the pH value of the wastewater to be 6.5-6.8, adding potassium dihydrogen phosphate, stirring, and sterilizing in a sterilization room at 120 ℃ to obtain a fermentation culture solution;
s5: adding various microorganism seed solutions into the fermentation culture solution obtained in the step S4, then sealing and fermenting to obtain fermentation liquor, centrifuging the fermentation liquor, standing, taking supernate, adding absolute ethyl alcohol, and stirring to obtain a microorganism flocculant;
s6: adding a natural polymeric flocculant into the microbial flocculant obtained in the step S4, adding distilled water, stirring, standing, centrifuging, precipitating, and drying in a vacuum environment and an ultraviolet illumination environment to obtain a composite biological flocculant;
s7: adding the composite biological flocculant obtained in the step S6 into the layered liquid obtained in the step S3, mixing and stirring uniformly, filtering, heating the obtained filtrate in a water bath, and concentrating in a vacuum environment to obtain purified zinc sulfate;
s8: and (5) cooling and crystallizing the purified zinc sulfate obtained in the step (S7), and drying after centrifugal separation to obtain the food-grade zinc sulfate.
Preferably, the molar mass ratio of the zinc sulfate to the distilled water in the step S1 is (1-1.5): (3-4), and in the step S1, stirring is controlled to be 30-45 min.
Preferably, the decoloring agent in the decoloring treatment in the step S2 is activated carbon, and the filter screen in the filtering treatment is 200 meshes.
Preferably, the composite extracting agent in the step S3 comprises, by volume percentage, 22.5-32.5% of tributyl phosphate, 17.5-19% of diisopropyl ether, 27.5-29% of methyl isobutyl ketone, and 21-29% of dinonyl naphthalene sulfonic acid, and the molar mass ratio of the composite extracting agent to the filtrate is 1: (3-4), in the step S3, the heating temperature of the water bath is 25-40 ℃, the stirring and shaking speed is 100-150r/min, and the oxidant is food-grade hydrogen peroxide.
Preferably, the content of the potassium dihydrogen phosphate in the step S4 is 3-3.5g/L, and meanwhile, the sodium arachidonic acid is added during stirring, and the content of the sodium arachidonic acid is 1.1g/30mL.
Preferably, the microbial seed liquid in the step S5 comprises Rhodococcus erythropolis, aspergillus fumigatus and Bacillus subtilis, the inoculation amount of each microorganism is 4-7%, the fermentation temperature is 25-35 ℃, the culture time is 60-80 h, and the molar mass ratio of the absolute ethyl alcohol to the supernatant in the step S5 is 1: (2.5-3.5).
Preferably, the natural polymer flocculant in step S6 is prepared by dissolving sodium hydroxide and tartaric acid solids in deionized water, adding an acrylamide monomer and a locust bean gum aqueous solution, stirring, then adjusting the pH of the reaction solution, charging nitrogen gas, then adding an initiator aqueous solution, sealing, irradiating with ultraviolet light, standing, washing, then purifying with N, N-dimethyl amide, drying at constant temperature until the quality is unchanged, and grinding to obtain a modified natural polymer flocculant, wherein the ultraviolet irradiation time in step S6 is 90-110nin.
Preferably, the molar mass ratio of the layering liquid to the composite bioflocculant in the step S7 is (1-1.5): (3.8-4.2), the heating temperature in the step S7 is controlled to be 80-90 ℃, and the vacuum concentration time is 1.5-2.5h.
Preferably, the cooling temperature in the step S8 is 20-25 ℃, and the cooling time is 2.5-3h.
The invention provides a method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material. The method has the following beneficial effects:
1. the preparation method disclosed by the invention is simple and efficient in preparation process and low in raw material price, and the food-grade zinc sulfate is produced by taking industrial-grade zinc sulfate as a raw material, so that the production cost of the food-grade zinc sulfate is greatly reduced, the preparation time is faster, the utilization rate of the raw material is high, and the yield is higher.
2. According to the invention, the prepared composite bioflocculant is added in the process of food-grade zinc sulfate, so that the produced product has higher edible safety, less pollution, energy conservation and environmental protection.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material, which comprises the following preparation steps:
s1: adding distilled water, stirring and fully mixing and dissolving to obtain a mixed solution;
s2: adding a decoloring agent into the mixed liquid obtained in the step S1 for decoloring, and then filtering to obtain a filtrate;
s3: adding a composite extracting agent and an oxidant into the filtrate obtained in the step S2, heating by adopting a water bath method, mixing, stirring and oscillating, standing for layering, and taking the upper-layer solution to obtain a layering solution for later use;
s4: taking a certain amount of bean curd wastewater, adjusting the pH value of the wastewater to be 6.5-6.8, adding potassium dihydrogen phosphate, stirring, and sterilizing in a sterilization chamber at 120 ℃ to obtain a fermentation culture solution;
s5: adding various microorganism seed solutions into the fermentation culture solution obtained in the step S4, then sealing and fermenting to obtain fermentation liquor, centrifuging the fermentation liquor, standing, taking supernate, adding absolute ethyl alcohol, and stirring to obtain a microorganism flocculant;
s6: adding a natural polymeric flocculant into the microbial flocculant obtained in the step S4, adding distilled water, stirring, standing, centrifuging, precipitating, and drying in a vacuum environment and an ultraviolet illumination environment to obtain a composite biological flocculant;
s7: adding the composite biological flocculant obtained in the step S6 into the layered liquid obtained in the step S3, mixing and stirring uniformly, filtering, heating the obtained filtrate in a water bath, and concentrating in a vacuum environment to obtain purified zinc sulfate;
s8: and (5) cooling and crystallizing the purified zinc sulfate obtained in the step (S7), and drying after centrifugal separation to obtain the food-grade zinc sulfate.
Further, the molar mass ratio of the zinc sulfate to the distilled water in the step S1 is (1-1.5): (3-4), and in the step S1, stirring is controlled to be 30-45 min.
Further, the decolorizing agent in the decolorizing treatment in the step S2 is activated carbon, and the filter screen for the filtering treatment is 200 meshes.
Further, in the step S3, the composite extracting agent includes, by volume percentage, 22.5-32.5% of tributyl phosphate, 17.5-19% of diisopropyl ether, 27.5-29% of methyl isobutyl ketone, and 21-29% of dinonyl naphthalene sulfonic acid, and the molar mass ratio of the composite extracting agent to the filtrate is 1: (3-4) in the step S3, the heating temperature of the water bath is 25-40 ℃, the stirring and shaking speed is 100-150r/min, and the oxidant is food-grade hydrogen peroxide.
Further, in the step S4, the content of the potassium dihydrogen phosphate is 3-3.5g/L, and meanwhile, the sodium arachidonic acid is added in the stirring process, and the content of the sodium dihydrogen phosphate is 1.1g/30mL.
Further, in the step S5, the microorganism seed solution comprises Rhodococcus erythropolis, aspergillus fumigatus and Bacillus subtilis, the inoculation amount of each microorganism is 4-7%, the fermentation temperature is 25-35 ℃, the culture time is 60-80 h, and the molar mass ratio of the absolute ethyl alcohol to the supernatant in the step S5 is 1: (2.5-3.5).
Further, the natural polymer flocculant in step S6 is prepared by dissolving sodium hydroxide and tartaric acid solid in deionized water, adding acrylamide monomer and locust bean gum aqueous solution, stirring, adjusting the pH of the reaction solution, charging nitrogen gas, adding initiator aqueous solution, sealing, irradiating with ultraviolet light, standing, washing, purifying with N, N-dimethyl amide, drying at constant temperature until the quality is unchanged, and grinding to obtain the modified natural polymer flocculant, wherein the ultraviolet irradiation time in step S6 is 90-110nin.
Further, the molar mass ratio of the layering liquid to the composite biological flocculant in the step S7 is (1-1.5): (3.8-4.2), the heating temperature in the step S7 is controlled to be 80-90 ℃, and the vacuum concentration time is 1.5-2.5h.
Further, the cooling temperature in the step S8 is 20-25 ℃, and the cooling time is 2.5-3h.
In the food-grade zinc sulfate obtained in the embodiment, the content of zinc sulfate heptahydrate is more than or equal to 105%, the content of alkaline earth metal is less than or equal to 0.05, the content of cadmium is less than or equal to 0.005, the content of lead is less than or equal to 0.004, the content of mercury is less than or equal to 0.003, the content of cadmium is less than or equal to 0.002, and the acidity is normal.
Example two:
the molar mass ratio of the zinc sulfate to the distilled water in the step S1 is (1.1-1.7): (2.5-4.5), and in the step S1, stirring is controlled to be 35-45 min.
The decolorizing agent in the decolorizing treatment in the step S2 is activated carbon, and the filter screen for filtering treatment is 200 meshes.
The composite extracting agent in the step S3 comprises 23-33% of tributyl phosphate, 15.5-18% of diisopropyl ether, 25.5-32.5% of methyl isobutyl ketone and 22-27% of dinonyl naphthalene sulfonic acid in percentage by volume, and the molar mass ratio of the composite extracting agent to the filtrate is 1: (2.5-3.5), in the step S3, the heating temperature of the water bath is 25-40 ℃, the stirring and shaking speed is 100-150r/min, and the oxidant is food-grade hydrogen peroxide.
In the step S4, the content of the potassium dihydrogen phosphate is 2.5-2.8g/L, and meanwhile, the sodium arachidonic acid is added in the stirring process, and the content of the sodium dihydrogen phosphate is 1.5g/30mL.
In the step S5, the microbial seed liquid comprises Rhodococcus erythropolis, aspergillus fumigatus and Bacillus subtilis, the inoculation amount of each microorganism is 5-8%, the fermentation temperature is 25-35 ℃, the culture time is 60-80 h, and the molar mass ratio of the absolute ethyl alcohol to the supernatant in the step S5 is 1: (3-3.5).
The natural polymer flocculant in the step S6 is prepared by dissolving sodium hydroxide and tartaric acid solid in deionized water, adding an acrylamide monomer and a locust bean gum aqueous solution, stirring, then adjusting the pH value of a reaction solution, filling nitrogen, then adding an initiator aqueous solution, sealing, irradiating by ultraviolet light, standing, washing, purifying by N, N-dimethyl amide, drying at constant temperature until the quality is unchanged, and grinding to obtain a modified natural polymer flocculant, wherein the ultraviolet irradiation time in the step S6 is 90-110nin.
The molar mass ratio of the layering liquid to the composite bioflocculant in the step S7 is (1-1.3): (3.5-4.5), the heating temperature in the step S7 is controlled to be 80-90 ℃, and the vacuum concentration time is 1.5-2.5h.
The cooling temperature in the step S8 is 20-25 ℃, and the cooling time is 2.5-3h.
In the food-grade zinc sulfate obtained in the embodiment, the content of zinc sulfate heptahydrate is more than or equal to 102.5%, the content of alkaline earth metal is less than or equal to 0.04, the content of cadmium is less than or equal to 0.01, the content of lead is less than or equal to 0.007, the content of mercury is less than or equal to 0.005, the content of cadmium is less than or equal to 0.1, and the acidity is normal.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various 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 (9)
1. A method for producing food-grade zinc sulfate by using industrial-grade zinc sulfate as a raw material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1: putting industrial zinc sulfate into a container, adding distilled water, stirring and fully mixing and dissolving to obtain a mixed solution;
s2: adding a decoloring agent into the mixed liquid obtained in the step S1 for decoloring, and then filtering to obtain a filtrate;
s3: adding a composite extracting agent and an oxidant into the filtrate obtained in the step S2, heating by adopting a water bath method, mixing, stirring and oscillating, standing for layering, and taking the upper layer solution to obtain a layering solution for later use;
s4: taking a certain amount of bean curd wastewater, adjusting the pH value of the wastewater to be 6.5-6.8, adding potassium dihydrogen phosphate, stirring, and sterilizing in a sterilization chamber at 120 ℃ to obtain a fermentation culture solution;
s5: adding various microorganism seed solutions into the fermentation culture solution obtained in the step S4, then sealing and fermenting to obtain fermentation liquor, centrifuging the fermentation liquor, standing, taking supernate, adding absolute ethyl alcohol, and stirring to obtain a microorganism flocculant;
s6: adding a natural polymeric flocculant into the microbial flocculant obtained in the step S4, adding distilled water, stirring, standing, centrifuging, precipitating, and drying in a vacuum environment and an ultraviolet illumination environment to obtain a composite biological flocculant;
s7: adding the composite biological flocculant obtained in the step S6 into the layered liquid obtained in the step S3, mixing and stirring uniformly, filtering, heating the obtained filtrate in a water bath, and concentrating in a vacuum environment to obtain purified zinc sulfate;
s8: and (5) cooling and crystallizing the purified zinc sulfate obtained in the step (S7), and drying after centrifugal separation to obtain the food-grade zinc sulfate.
2. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, characterized by comprising the following steps: the molar mass ratio of the zinc sulfate to the distilled water in the step S1 is (1-1.5): (3-4), in the step S1, stirring is controlled to be 30-45 min.
3. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, wherein the method comprises the following steps: the decolorizing agent in the decolorizing treatment in the step S2 is activated carbon, and the filter screen for filtering treatment is 200 meshes.
4. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, wherein the method comprises the following steps: the composite extracting agent in the step S3 comprises 22.5-32.5% of tributyl phosphate, 17.5-19% of diisopropyl ether, 27.5-29% of methyl isobutyl ketone and 21-29% of dinonyl naphthalene sulfonic acid in percentage by volume, the molar mass ratio of the composite extracting agent to the filtrate is 1 (3-4), the heating temperature of the water bath in the step S3 is 25-40 ℃, the stirring and shaking speed is 100-150r/min, and the oxidizing agent is food-grade hydrogen peroxide.
5. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, wherein the method comprises the following steps: in the step S4, the content of the potassium dihydrogen phosphate is 3-3.5g/L, and meanwhile, the sodium arachidonic acid is added in the stirring process, and the content of the sodium dihydrogen phosphate is 1.1g/30mL.
6. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, characterized by comprising the following steps: the microbial seed liquid in the step S5 comprises Rhodococcus erythropolis, aspergillus fumigatus and Bacillus subtilis, the inoculation amount of each microorganism is 4-7%, the fermentation temperature is 25-35 ℃, the culture time is 60-80 h, and the molar mass ratio of the absolute ethyl alcohol to the supernatant in the step S5 is 1: (2.5-3.5).
7. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, wherein the method comprises the following steps: the natural polymer flocculant in the step S6 is prepared by dissolving sodium hydroxide and tartaric acid solids in deionized water, adding an acrylamide monomer and a locust bean gum aqueous solution, stirring, then adjusting the pH value of a reaction solution, filling nitrogen, then adding an initiator aqueous solution, sealing, irradiating by ultraviolet light, standing, washing, purifying by N, N-dimethyl amide, drying at constant temperature until the quality is unchanged, and grinding to obtain a modified natural polymer flocculant, wherein the ultraviolet irradiation time in the step S6 is 90-110nin.
8. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, wherein the method comprises the following steps: the molar mass ratio of the layering liquid to the composite bioflocculant in the step S7 is (1-1.5): (3.8-4.2), the heating temperature in the step S7 is controlled to be 80-90 ℃, and the vacuum concentration time is 1.5-2.5h.
9. The method for producing food-grade zinc sulfate from industrial-grade zinc sulfate according to claim 1, wherein the method comprises the following steps: the cooling temperature in the step S8 is 20-25 ℃, and the cooling time is 2.5-3h.
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| CA2878386A1 (en) * | 2012-07-23 | 2014-01-30 | Butamax Advanced Biofuels Llc | Method for mitigating the formation of a rag layer in a fermentable carbon source |
| CN104341001A (en) * | 2013-08-07 | 2015-02-11 | 宜昌瑞特精细化工有限公司 | Method for producing food-grade zinc sulfate with industrial-grade zinc sulfate as raw material |
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| CN111995026A (en) * | 2020-06-28 | 2020-11-27 | 嘉兴市爵拓科技有限公司 | Environment-friendly efficient composite biological flocculant and preparation method thereof |
| CN112624179A (en) * | 2021-02-03 | 2021-04-09 | 浙江爱科新材料有限公司 | Preparation method of high-purity homogeneous zinc sulfate heptahydrate |
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| CA2878386A1 (en) * | 2012-07-23 | 2014-01-30 | Butamax Advanced Biofuels Llc | Method for mitigating the formation of a rag layer in a fermentable carbon source |
| CN104341001A (en) * | 2013-08-07 | 2015-02-11 | 宜昌瑞特精细化工有限公司 | Method for producing food-grade zinc sulfate with industrial-grade zinc sulfate as raw material |
| CN107385216A (en) * | 2017-07-20 | 2017-11-24 | 台山市化工厂有限公司 | The method that monohydrate zinc sulphate is prepared from utilising zinc containing waste residue |
| CN108726499A (en) * | 2018-08-01 | 2018-11-02 | 蒋华民 | A kind of food-grade calcium hydrogen phosphate and preparation method thereof |
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