CN115676871A - Preparation process of nano copper oxide powder - Google Patents
Preparation process of nano copper oxide powder Download PDFInfo
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- CN115676871A CN115676871A CN202211376814.6A CN202211376814A CN115676871A CN 115676871 A CN115676871 A CN 115676871A CN 202211376814 A CN202211376814 A CN 202211376814A CN 115676871 A CN115676871 A CN 115676871A
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- oxide powder
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 71
- 239000005751 Copper oxide Substances 0.000 claims abstract description 27
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 27
- 239000000654 additive Substances 0.000 claims abstract description 26
- 230000000996 additive effect Effects 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 58
- 238000003756 stirring Methods 0.000 claims description 45
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 40
- 229920002498 Beta-glucan Polymers 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 31
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 25
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 22
- 229960001484 edetic acid Drugs 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000004108 freeze drying Methods 0.000 claims description 11
- 238000002390 rotary evaporation Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- -1 sodium tetrahydroborate Chemical compound 0.000 claims description 7
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide Chemical compound CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 claims description 6
- 238000000502 dialysis Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229950005499 carbon tetrachloride Drugs 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 5
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000002195 synergetic effect Effects 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 2
- 229960004643 cupric oxide Drugs 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000012043 crude product Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920001732 Lignosulfonate Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- 150000004699 copper complex Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the technical field of nano materials, in particular to a preparation process of nano copper oxide powder; the reaction additive finished product prepared by the invention is applied to the preparation process of the nano copper oxide powder, so that the dispersion performance of the nano copper oxide powder in a reaction liquid can be effectively improved, the agglomeration phenomenon of the nano copper oxide powder is reduced, the particle size of the prepared nano copper oxide powder can be effectively controlled, the appearance of the nano copper oxide powder is more uniform, and the grade of the nano copper oxide powder is better; meanwhile, the yield of the nano copper oxide powder is relatively high; in addition, the invention effectively reduces the impurity content in the prepared nano copper oxide product finally through the cooperative coordination of the procedures of washing treatment, vacuum freeze drying, high-temperature sintering and the like, obviously improves the purity of the prepared nano copper oxide powder and ensures the product quality and grade.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation process of nano copper oxide powder.
Background
The nano copper oxide is a black metal oxide and is widely applied to various fields as an important inorganic material. In recent years, due to the abnormal characteristics of copper-containing oxides in the field of high-temperature superconductivity, copper oxide becomes an important model compound for explaining the spectral characteristics of complex oxides; in the aspect of the sensor, due to the peculiar characteristics of the copper oxide nano particles, the copper oxide nano particles are very sensitive to external environments such as temperature, light, moisture and the like, so that the response speed, the sensitivity and the selectivity of the sensor can be greatly improved; the nano copper oxide has good catalytic action on chemical reactions such as complete oxidation of toluene and ethanol, synthesis of phenol from benzene and the like; in the battery industry, nano copper oxide can be used as an anode material of a high-performance lithium battery and a cathode material of a solar battery. In addition, the nano copper oxide powder has good application prospects in the aspects of superconductivity, sensors, chemical catalysis, batteries and the like, and can be predicted to have great application potential and market prospects in many fields.
At present, the preparation method of the nano copper oxide powder mainly comprises a solid phase method and a liquid phase method. The solid phase method is a traditional powder process, in which metal salts or metal oxides are fully mixed according to a formula, and are ground to fully react to directly obtain nano copper oxide powder, or are calcined and ground to obtain ultrafine powder. The powder particles prepared by the method have the advantages of no agglomeration, good filling property, low cost, high yield, simple preparation process and the like, and the method is still a common method so far, but has the defects of high energy consumption, low efficiency, low fineness of the powder, easy impurity mixing and the like. The liquid phase method is to select one or more soluble copper salts, prepare solution according to the prepared material composition, make each element present ion or molecular state, then select a proper precipitator or use operations such as evaporation, sublimation, hydrolysis, etc., make copper ion precipitate or crystallize out evenly, finally precipitate or crystallize to get nanometer cupric oxide powder after heat treatment. The method has the advantages of good metal selectivity, high recovery rate, renewable reagents, easy serialization and the like, and is the most extensive method for preparing the nano copper oxide powder in laboratories and industries at present.
The invention patent with the publication number of CN 103420408A provides a preparation method of nano copper oxide, which comprises the following steps: the method comprises the steps of taking lignosulfonate as a template, carrying out solid-phase reaction on copper salt and sodium hydroxide, and calcining at different temperatures to remove the template to prepare the nano copper oxide. The lignosulfonate is a byproduct of pulping by a sulfurous acid method, contains rich functional groups, has good diffusivity, realizes a controllable technology of a nano material by using the lignosulfonate as a template agent, fully utilizes waste resources and reduces pollution to the environment. The nano copper oxide synthesized by the solid phase method has the advantages of simple synthesis process, low cost, high yield, short time and less environmental pollution. But the synthesized nano copper oxide has various shapes and poorer size and granularity uniformity.
The invention patent with the publication number of CN 113955795A provides a preparation method of nano copper oxide, which comprises the following steps: preparing 0.01mol/L copper nitrate aqueous solution; preparing 3mol/L polyvinylpyrrolidone aqueous solution; mixing 0.01mol/L copper nitrate aqueous solution and 3mol/L polyvinylpyrrolidone aqueous solution, and heating to react at 40-70 ℃ to obtain a copper complex; dripping the copper complex into the mixed alkaline water solution, and stirring for reaction to obtain a crude product of the nano copper oxide; and centrifuging the crude product of the nano copper oxide to obtain a precipitate, drying the precipitate in an oven, and cooling to room temperature to obtain a finished product of the nano copper oxide. The preparation method is simple to operate, mild in reaction conditions, low in production cost and environment-friendly, and the prepared nano copper oxide is good in shape and can react at a lower temperature. But the nano copper oxide product prepared by the method has more impurities and relatively low purity, and needs to be further improved!
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process of nano copper oxide powder, the prepared nano copper oxide powder has better dispersion performance and is not easy to agglomerate, the particle size of the prepared nano copper oxide powder is effectively controlled, and the nano copper oxide powder has more uniform appearance and better grade; in addition, the impurities contained in the product are better, and the product quality and the product grade are ensured.
The invention is realized by the following technical scheme:
a preparation process of nano copper oxide powder comprises the following steps:
step one, according to 1: 1.2-1.8, respectively mixing and dispersing a copper nitrate aqueous solution with the concentration of 0.5-0.8 g/mL and a reaction additive aqueous solution with the concentration of 0.7-1.2 g/mL uniformly, adjusting the pH of the mixture to 9.5-10.8 by using ammonia water while stirring, then raising the temperature of the obtained mixed solution to 30-40 ℃, and stirring and reacting for 50-80 min at the temperature; after the reaction is finished, storing the obtained reaction product for later use;
step two, adding cyclohexane into the reaction kettle, stirring at the speed of 150-200 r/min, and heating to 55-65 ℃ after stirring for 10-20 min; then adding a dispersant with the mass 0.5-0.65 time of that of the reaction additive, a synergistic dispersant with the volume 1.8-2.5 percent of cyclohexane and a reaction product obtained in the step one with the volume 2.5-3.5 percent, mixing and stirring for 5-8 h, and storing the obtained colloidal particles for later use;
step three, freezing the colloidal particles obtained in the step two at a low temperature of-25 to-5 ℃, then carrying out low-temperature suction filtration on the colloidal particles, and washing the colloidal particles after the suction filtration is finished; after washing, carrying out vacuum freeze drying treatment for 25-30 h at the temperature of-55 to-40 ℃, transferring the copper oxide powder into sintering equipment for high-temperature sintering treatment after drying, and finally obtaining the finished product of the nano copper oxide.
Still further, the method for preparing the reactive additive comprises the following steps:
putting beta-1,3-glucan into N, N-dimethylformamide with the mass 5-8 times of that of the beta-1,3-glucan, stirring and dissolving the beta-1,3-glucan under the condition of an oil bath at the temperature of 80-90 ℃, and preserving heat for reacting for 30-40 min after the beta-1,3-glucan is fully dissolved; after the reaction is finished, adding sodium azide with the mass of 3.0 to 3.5 times of that of the beta-1,3-glucan into the obtained product component, mechanically and uniformly mixing, then respectively adding phenyl triphenolate with the mass of 0.4 to 0.6 percent of the beta-1,3-glucan and 1.5 to 3 times of tetrachloromethane into the mixture, and carrying out heat preservation reaction for 40 to 60min at the temperature of between 80 and 90 ℃; after the reaction is finished, carrying out precipitation treatment on the precipitate by using methanol, then carrying out centrifugal washing on the obtained precipitate for 2-3 times by using methanol, ethanol and deionized water respectively, and then carrying out drying treatment, wherein the obtained solid micro powder is stored for later use;
II, dissolving the solid micro powder obtained in the step I in dimethyl sulfoxide according to a solid-to-liquid ratio of 0.08-0.15 g/mL, then adding sodium tetrahydroborate with the molar weight of 0.08-0.15 time of that of the dimethyl sulfoxide, stirring and reacting for 10-20 hours in an oil bath kettle at the temperature of 60-75 ℃, after the reaction is finished, adding absolute ethyl alcohol with the volume of 0.3-0.6 time of that of the dimethyl sulfoxide, and continuing to react for 3-5 hours; performing centrifugal separation on the obtained product components, performing dialysis treatment on the product components for 2 to 4 days, and finally performing rotary evaporation and freeze drying on the product components to obtain product powder for storage and standby;
III, dissolving a proper amount of ethylene diamine tetraacetic acid into dimethyl sulfoxide according to the dosage ratio of 0.06-0.12 g/mL, adding a proper amount of mixed components, respectively adding N, N-diisopropylethylamine with the molar weight 0.9-1.3 times that of the ethylene diamine tetraacetic acid and product powder with the mass 0.55-0.75 times that of the ethylene diamine tetraacetic acid after uniformly mixing and dispersing, continuously introducing nitrogen into the mixture, and carrying out heat preservation reaction at the temperature of 50-65 ℃ for 60-80 hours; and after the reaction is finished, purifying the reaction product to obtain a finished product of the reaction additive.
Further, stirring the ammonia water at a stirring speed of 800-1200 r/min when the ammonia water is added in the step one, wherein the concentration of the ammonia water solution is 6-8 mol/L; the dropping speed of the ammonia water is 3-8 mL/min.
Furthermore, the mixed component in the step III is compounded by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and N-hydroxysuccinimide, and the dosage of the mixed component and the N-hydroxysuccinimide is 1.0-1.5 times and 1.2-1.4 times of the molar weight of the ethylenediamine tetraacetic acid respectively.
Furthermore, the dispersant used in the second step is any one of cetyltrimethylammonium chloride and cetyltrimethylammonium bromide.
Further, the synergistic dispersant used in the second step is n-butanol.
Furthermore, in the washing process of the third step, absolute ethyl alcohol with the temperature of-18 to-15 ℃ is adopted for washing, and the washing times are 3 to 4.
Furthermore, the sintering temperature during the high-temperature sintering in the third step is set to be 450-550 ℃, and the sintering time is set to be 3-5 h.
Further, the purification treatment process in step iii is: firstly, dialyzing in a distillation environment, and then carrying out rotary evaporation and freeze-drying treatment on the mixture.
The invention has the beneficial effects that:
the invention takes beta-1,3-glucan, sodium azide, triphenol phenyl ester and the like as starting raw materials to prepare the solid micro powder by chemical reaction. Then the solid micro powder, sodium tetrahydroborate and the like are used as raw materials, the raw materials and the raw materials are subjected to chemical reaction to claim a crude product of the product powder, and the crude product of the product powder is subjected to the matched use of working procedures such as centrifugal separation, rotary evaporation and freeze drying of a dialysis machine and the like, so that a finished product of the product powder is finally prepared. Then the prepared product powder and ethylene diamine tetraacetic acid, 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide, N-hydroxysuccinimide and the like are used as raw materials, and a reaction additive finished product is finally prepared through the generated chemical reaction. The prepared reaction additive finished product is applied to the preparation process of the nano copper oxide powder, so that the dispersion performance of the nano copper oxide powder in a reaction liquid can be effectively improved, the agglomeration phenomenon of the nano copper oxide powder is reduced, the particle size of the prepared nano copper oxide powder can be effectively controlled, the appearance of the nano copper oxide powder is more uniform, and the grade of the nano copper oxide powder is better. Meanwhile, the yield of the nano copper oxide powder is relatively high. In addition, the invention effectively reduces the impurity content in the prepared nano copper oxide product finally through the cooperative coordination of the procedures of washing treatment, vacuum freeze drying, high-temperature sintering and the like, obviously improves the purity of the prepared nano copper oxide powder and ensures the product quality and grade.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an SEM image of the nano-copper oxide powder prepared by the present invention;
FIG. 2 is a high power SEM image of the SEM image of FIG. 1 at a first viewing angle;
FIG. 3 is a second SEM image of the SEM image of FIG. 1 at a high magnification.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. 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
A preparation process of nano copper oxide powder comprises the following steps:
step one, according to 1:1.2, respectively mixing and dispersing a copper nitrate aqueous solution with the concentration of 0.5g/mL and a reaction additive aqueous solution with the concentration of 0.7g/mL uniformly in a volume ratio, adjusting the pH value to 9.5 by using ammonia water while stirring, then raising the temperature of the obtained mixed solution to 30 ℃, and stirring and reacting for 50min at the temperature; after the reaction is finished, storing the obtained reaction product for later use; wherein, when ammonia water is added, the ammonia water is stirred at the stirring speed of 800r/min, and the concentration of the ammonia water solution is 6mol/L; the dropping speed of the ammonia water is 3mL/min
Step two, adding cyclohexane into the reaction kettle, stirring at the speed of 150r/min, stirring for 10-20 min, and heating to 55 ℃; then adding hexadecyl trimethyl ammonium chloride with the mass being 0.5 time of that of the reaction additive, n-butyl alcohol with the volume being 1.8 percent of cyclohexane and a reaction product with the volume being 2.5 percent of that of the first step into the mixture, mixing and stirring the mixture for 5 hours, and then storing the obtained colloidal particles for later use;
step three, freezing the colloidal particles obtained in the step two at a low temperature of-25 ℃, then carrying out low-temperature suction filtration on the colloidal particles, and washing the colloidal particles for 3 times by using absolute ethyl alcohol at a temperature of-18 ℃ after the suction filtration is finished; after washing, carrying out vacuum freeze drying treatment for 25h at-55 ℃, transferring the copper oxide powder into sintering equipment after drying, and sintering the copper oxide powder for 3h at 450 ℃, thus obtaining the finished product of the nano copper oxide.
The preparation method of the reaction additive comprises the following steps:
putting beta-1,3-glucan into N, N-dimethylformamide with the mass 5 times of that of the beta-1,3-glucan, stirring and dissolving the beta-1,3-glucan under the condition of an oil bath at 80 ℃, and preserving heat for reacting for 30min after the beta-1,3-glucan is fully dissolved; after the reaction is finished, adding sodium azide with the mass of 3.0 times of that of the beta-1,3-glucan into the obtained product component, mechanically and uniformly mixing, then respectively adding phenyl triphenolate with the mass of 0.4% of that of the beta-1,3-glucan and 1.5 times of tetrachloromethane into the mixture, and carrying out heat preservation reaction for 40min at the temperature of 80 ℃; after the reaction is finished, carrying out precipitation treatment on the precipitate by using methanol, then respectively carrying out centrifugal washing on the obtained precipitate for 2 times by using methanol, ethanol and deionized water, and then carrying out drying treatment, wherein the obtained solid micro powder is stored for later use;
II, dissolving the solid micro powder obtained in the step I in dimethyl sulfoxide according to a solid-to-liquid ratio of 0.08g/mL, adding sodium tetrahydroborate with the molar quantity being 0.08 times of that of the dimethyl sulfoxide, stirring and reacting for 10 hours in an oil bath kettle at the temperature of 60 ℃, adding absolute ethyl alcohol with the volume being 0.3 times of that of the dimethyl sulfoxide into the mixture after the reaction is finished, and continuing to react for 3 hours; performing centrifugal separation on the obtained product components, performing dialysis treatment on the product components for 2 days, and finally performing rotary evaporation and freeze drying on the product components to obtain product powder for storage and standby;
III, dissolving a proper amount of ethylene diamine tetraacetic acid into dimethyl sulfoxide according to the dosage ratio of 0.06g/mL, adding a proper amount of mixed components, respectively adding N, N-diisopropylethylamine with the molar weight 0.9 time that of the ethylene diamine tetraacetic acid and product powder with the mass 0.55 time that of the ethylene diamine tetraacetic acid into the mixture after uniformly mixing and dispersing, then continuously introducing nitrogen into the mixture, and carrying out heat preservation reaction at the temperature of 50 ℃ for 60 hours; after the reaction is finished, firstly dialyzing the mixture in a distillation environment, and then carrying out rotary evaporation and freeze-drying treatment on the mixture to finally obtain a reaction additive finished product; wherein the mixed components are compounded by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide with the molar weight equal to that of the ethylene diamine tetraacetic acid and N-hydroxysuccinimide with the molar weight 1.2 times that of the ethylene diamine tetraacetic acid.
Example 2
A preparation process of nano copper oxide powder comprises the following steps:
step one, according to 1:1.5, respectively mixing and uniformly dispersing a copper nitrate aqueous solution with the concentration of 0.6g/mL and a reaction additive aqueous solution with the concentration of 1.0g/mL according to the volume ratio, adjusting the pH value to 10.3 by using ammonia water while stirring, then raising the temperature of the obtained mixed solution to 35 ℃, and stirring and reacting for 70min at the temperature; after the reaction is finished, storing the obtained reaction product for later use; stirring the ammonia water at a stirring speed of 1000r/min when the ammonia water is added, wherein the concentration of the ammonia water solution is 7mol/L; the dropping speed of the ammonia water is 5mL/min;
step two, adding cyclohexane into the reaction kettle, stirring at the speed of 180r/min, stirring for 15min, and heating to 60 ℃; then adding cetyl trimethyl ammonium bromide with the mass being 0.6 time of that of the reaction additive, n-butanol with the volume being 2.0 percent of cyclohexane and a reaction product obtained in the step one with the volume being 3.0 percent of cyclohexane into the mixture, mixing and stirring the mixture for 6 hours, and storing the obtained colloidal particles for later use;
step three, freezing the colloidal particles obtained in the step two at a low temperature of-15 ℃, then carrying out low-temperature suction filtration on the colloidal particles, and washing the colloidal particles for 3 times by using absolute ethyl alcohol at the temperature of-16 ℃ after the suction filtration is finished; after washing, carrying out vacuum freeze drying treatment for 28h at-45 ℃, after drying, transferring the copper oxide to sintering equipment, and sintering at 500 ℃ for 4h to obtain the finished product of the nano copper oxide.
The preparation method of the reaction additive comprises the following steps:
putting beta-1,3-glucan into N, N-dimethylformamide with the mass 6 times of that of the beta-1,3-glucan, stirring and dissolving the beta-1,3-glucan under the condition of an oil bath at 85 ℃, and preserving heat for reacting for 35min after the beta-1,3-glucan is fully dissolved; after the reaction is finished, adding sodium azide which is 3.2 times of that of beta-1,3-glucan into the obtained product component, mechanically and uniformly mixing, then respectively adding phenyl triphenolate which is 0.5 percent of that of beta-1,3-glucan and 2.5 times of tetrachloromethane into the product component, and carrying out heat preservation reaction for 50min at the temperature of 85 ℃; after the reaction is finished, carrying out precipitation treatment on the precipitate by using methanol, then respectively carrying out centrifugal washing on the obtained precipitate by using methanol, ethanol and deionized water for 3 times, and then carrying out drying treatment, wherein the obtained solid micro powder is stored for later use;
II, dissolving the solid micro powder obtained in the step I in dimethyl sulfoxide according to a solid-to-liquid ratio of 0.1g/mL, adding sodium tetrahydroborate with the molar weight being 0.12 times that of the dimethyl sulfoxide, stirring and reacting for 15 hours in an oil bath kettle at the temperature of 70 ℃, adding absolute ethyl alcohol with the volume being 0.5 times that of the dimethyl sulfoxide into the mixture after the reaction is finished, and continuing to react for 4 hours; performing centrifugal separation on the obtained product components, performing dialysis treatment on the product components for 3 days, and finally performing rotary evaporation and freeze drying on the product components to obtain product powder for storage and standby;
III, dissolving a proper amount of ethylene diamine tetraacetic acid into dimethyl sulfoxide according to the dosage ratio of 0.09g/mL, adding a proper amount of mixed components, respectively adding N, N-diisopropylethylamine with the molar quantity 1.2 times that of the ethylene diamine tetraacetic acid and product powder with the mass 0.65 times that of the ethylene diamine tetraacetic acid into the mixture after uniformly mixing and dispersing, then continuously introducing nitrogen into the mixture, and carrying out heat preservation reaction at the temperature of 60 ℃ for 70 hours; after the reaction is finished, firstly dialyzing the mixture in a distillation environment, and then carrying out rotary evaporation freeze-drying treatment on the mixture to finally obtain a reaction additive finished product; wherein, the mixed component in the step III is compounded by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and N-hydroxysuccinimide, and the dosage of the two components is respectively 1.2 times and 1.3 times of the molar weight of the ethylenediamine tetraacetic acid.
Example 3
A preparation process of nano copper oxide powder comprises the following steps:
step one, according to 1:1.8, respectively mixing and uniformly dispersing a copper nitrate aqueous solution with the concentration of 0.8g/mL and a reaction additive aqueous solution with the concentration of 1.2g/mL according to the volume ratio, adjusting the pH value to 10.8 by using ammonia water while stirring, then raising the temperature of the obtained mixed solution to 40 ℃, and stirring and reacting for 80min at the temperature; after the reaction is finished, storing the obtained reaction product for later use; stirring the ammonia water at a stirring speed of 1200r/min when the ammonia water is added, wherein the concentration of the ammonia water solution is 8mol/L; the dropping speed of the ammonia water is 8mL/min;
step two, adding cyclohexane into the reaction kettle, stirring at the speed of 200r/min, and heating to 65 ℃ after stirring for 20 min; then adding hexadecyl trimethyl ammonium chloride with the mass being 0.65 time of that of the reaction additive, n-butyl alcohol with the volume being 2.5 percent of cyclohexane and a reaction product obtained in the step one with the volume being 3.5 percent respectively, mixing and stirring for 8 hours, and storing the obtained colloidal particles for later use;
step three, freezing the colloidal particles obtained in the step two at a low temperature of-5 ℃, then carrying out low-temperature suction filtration on the colloidal particles, and washing the colloidal particles for 4 times by using absolute ethyl alcohol at a temperature of-15 ℃ after the suction filtration is finished; after washing, carrying out vacuum freeze drying treatment for 30h at-40 ℃, transferring the copper oxide powder to sintering equipment for sintering for 5h at 550 ℃ after drying, and finally obtaining the finished product of the nano copper oxide.
The preparation method of the reaction additive comprises the following steps:
putting beta-1,3-glucan into N, N-dimethylformamide with the mass 8 times of that of the beta-1,3-glucan, stirring and dissolving the beta-1,3-glucan under the condition of 90 ℃ in oil bath, and preserving heat for reacting for 40min after the beta-1,3-glucan is fully dissolved; after the reaction is finished, adding sodium azide which is 3.5 times of that of beta-1,3-glucan into the obtained product component, mechanically and uniformly mixing, then respectively adding phenyl triphenolate which is 0.6 percent of that of beta-1,3-glucan and 3 times of tetrachloromethane into the mixture, and carrying out heat preservation reaction for 60min at the temperature of 90 ℃; after the reaction is finished, carrying out precipitation treatment on the precipitate by using methanol, then respectively carrying out centrifugal washing on the obtained precipitate by using methanol, ethanol and deionized water for 3 times, and then carrying out drying treatment, wherein the obtained solid micro powder is stored for later use;
II, dissolving the solid micro powder obtained in the step I in dimethyl sulfoxide according to a solid-to-liquid ratio of 0.15g/mL, adding sodium tetrahydroborate with the molar quantity being 0.15 times of that of the dimethyl sulfoxide, stirring and reacting for 20 hours in an oil bath kettle at the temperature of 75 ℃, adding absolute ethyl alcohol with the volume being 0.6 times of that of the dimethyl sulfoxide after the reaction is finished, and continuing to react for 5 hours; performing centrifugal separation on the obtained product components, performing dialysis treatment on the product components for 4 days, and finally performing rotary evaporation and freeze drying on the product components to obtain product powder for storage and standby;
III, dissolving a proper amount of ethylene diamine tetraacetic acid into dimethyl sulfoxide according to the dosage ratio of 0.12g/mL, adding a proper amount of mixed components, respectively adding N, N-diisopropylethylamine with the molar weight 1.3 times that of the ethylene diamine tetraacetic acid and product powder with the mass 0.75 times that of the ethylene diamine tetraacetic acid into the mixture after uniformly mixing and dispersing, then continuously introducing nitrogen into the mixture, and carrying out heat preservation reaction for 80 hours at the temperature of 65 ℃; after the reaction is finished, firstly dialyzing the mixture in a distillation environment, and then carrying out rotary evaporation and freeze-drying treatment on the mixture to finally obtain a reaction additive finished product; wherein the mixed component is compounded by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and N-hydroxysuccinimide, and the dosage of the two components is 1.5 times and 1.4 times of the molar weight of the ethylenediamine tetraacetic acid respectively.
Comparative example 1: the preparation process of the nano copper oxide powder provided in the embodiment is substantially the same as that of the embodiment 1, and the main differences are as follows: in this example, an equal amount of citric acid was used in place of the reaction additive.
Comparative example 2: the preparation process of the nano copper oxide powder provided in the embodiment is substantially the same as that of the embodiment 1, and the main differences are as follows: in this example, the same amount of malic acid was used in place of the reaction additive.
Comparative example 3: the preparation process of the nano copper oxide powder provided in the embodiment is substantially the same as that of the embodiment 1, and the main differences are as follows: in this example, an equal amount of tartaric acid was used in place of the reaction additive.
And (3) sample testing: the nano copper oxide powder samples prepared in examples 1 to 3 and comparative examples 1 to 3 were tested, and the test data are recorded in the following table:
| nano copper oxide particle size/nm | Yield/% of nano-copper oxide | Purity/% of nano copper oxide | |
| Example 1 | 68 | 98.9 | 99.52 |
| Example 2 | 62 | 98.7 | 99.63 |
| Example 3 | 73 | 97.2 | 99.57 |
| Comparative example 1 | 112 | 87.6 | 93.6 |
| Comparative example 2 | 116 | 85.3 | 93.9 |
| Comparative example 3 | 122 | 86.8 | 92.8 |
The relevant data in the comparison and analysis table shows that the detection shows that the prepared nano copper oxide powder has better dispersion performance and is not easy to agglomerate, the particle size of the prepared nano copper oxide powder is effectively controlled, and the nano copper oxide powder has more uniform appearance and better grade; in addition, the impurities contained in the product are better, and the product quality and the product grade are ensured. Therefore, the preparation process of the nano copper oxide powder provided by the invention has wider market prospect and is more suitable for popularization.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A preparation process of nano copper oxide powder is characterized by comprising the following steps:
step one, according to 1: 1.2-1.8, respectively mixing and dispersing a copper nitrate aqueous solution with the concentration of 0.5-0.8 g/mL and a reaction additive aqueous solution with the concentration of 0.7-1.2 g/mL uniformly, adjusting the pH of the mixture to 9.5-10.8 by using ammonia water while stirring, then raising the temperature of the obtained mixed solution to 30-40 ℃, and stirring and reacting for 50-80 min at the temperature; after the reaction is finished, storing the obtained reaction product for later use;
step two, adding cyclohexane into the reaction kettle, stirring at the speed of 150-200 r/min, and heating to 55-65 ℃ after stirring for 10-20 min; then adding a dispersant with the mass 0.5-0.65 time of that of the reaction additive, a synergistic dispersant with the volume 1.8-2.5 percent of cyclohexane and a reaction product obtained in the step one with the volume 2.5-3.5 percent, mixing and stirring for 5-8 h, and storing the obtained colloidal particles for later use;
step three, freezing the colloidal particles obtained in the step two at a low temperature of-25 to-5 ℃, then carrying out low-temperature suction filtration on the colloidal particles, and washing the colloidal particles after the suction filtration is finished; after washing, carrying out vacuum freeze drying treatment for 25-30 h at the temperature of-55 to-40 ℃, transferring the copper oxide powder into sintering equipment for high-temperature sintering treatment after drying, and finally obtaining the finished product of the nano copper oxide.
2. The preparation process of nano copper oxide powder according to claim 1, wherein the preparation method of the reaction additive comprises the following steps:
i, putting beta-1,3-glucan into N, N-dimethylformamide with the mass 5-8 times of that of the beta-1,3-glucan, stirring and dissolving the beta-1,3-glucan under the condition of an oil bath at the temperature of 80-90 ℃, and preserving heat for reacting for 30-40 min after the beta-1,3-glucan is fully dissolved; after the reaction is finished, adding sodium azide with the mass of 3.0 to 3.5 times of that of the beta-1,3-glucan into the obtained product component, mechanically and uniformly mixing, then respectively adding phenyl triphenolate with the mass of 0.4 to 0.6 percent of the beta-1,3-glucan and 1.5 to 3 times of tetrachloromethane into the mixture, and carrying out heat preservation reaction for 40 to 60min at the temperature of between 80 and 90 ℃; after the reaction is finished, carrying out precipitation treatment on the precipitate by using methanol, then carrying out centrifugal washing on the obtained precipitate for 2-3 times by using methanol, ethanol and deionized water respectively, and then carrying out drying treatment, wherein the obtained solid micro powder is stored for later use;
II, dissolving the solid micro powder obtained in the step I in dimethyl sulfoxide according to a solid-to-liquid ratio of 0.08-0.15 g/mL, adding sodium tetrahydroborate with the molar quantity of 0.08-0.15 times that of the dimethyl sulfoxide, stirring and reacting for 10-20 hours in an oil bath kettle at the temperature of 60-75 ℃, adding absolute ethyl alcohol with the volume of 0.3-0.6 times that of the dimethyl sulfoxide after the reaction is finished, and continuing to react for 3-5 hours; performing centrifugal separation on the obtained product components, performing dialysis treatment on the product components for 2 to 4 days, and finally performing rotary evaporation and freeze drying on the product components to obtain product powder for storage and standby;
III, dissolving a proper amount of ethylene diamine tetraacetic acid into dimethyl sulfoxide according to the dosage ratio of 0.06-0.12 g/mL, adding a proper amount of mixed components, respectively adding N, N-diisopropylethylamine with the molar weight 0.9-1.3 times of that of the ethylene diamine tetraacetic acid and product powder with the mass 0.55-0.75 times of that of the ethylene diamine tetraacetic acid after uniformly mixing and dispersing, continuously introducing nitrogen into the mixture, and carrying out heat preservation reaction at the temperature of 50-65 ℃ for 60-80 hours; and after the reaction is finished, purifying the reaction product to obtain a finished product of the reaction additive.
3. The process for preparing nano copper oxide powder according to claim 1, wherein the process comprises the following steps: stirring the ammonia water at the stirring speed of 800-1200 r/min when the ammonia water is added in the first step, wherein the concentration of the ammonia water solution is 6-8 mol/L; the dropping speed of the ammonia water is 3-8 mL/min.
4. The preparation process of the nano copper oxide powder according to claim 2, wherein the preparation process comprises the following steps: and the mixed component in the step III is compounded by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide and N-hydroxysuccinimide, and the dosage of the mixed component and the N-hydroxysuccinimide is 1.0-1.5 times and 1.2-1.4 times of the molar weight of the ethylenediamine tetraacetic acid respectively.
5. The preparation process of the nano copper oxide powder according to claim 1, wherein the preparation process comprises the following steps: and the dispersant used in the second step is any one of hexadecyl trimethyl ammonium chloride and hexadecyl trimethyl ammonium bromide.
6. The process for preparing nano copper oxide powder according to claim 1, wherein the process comprises the following steps: and the synergistic dispersant used in the second step is n-butyl alcohol.
7. The preparation process of the nano copper oxide powder according to claim 1, wherein the preparation process comprises the following steps: and in the washing process of the third step, absolute ethyl alcohol with the temperature of-18 to-15 ℃ is adopted for washing, and the washing times are 3 to 4.
8. The preparation process of the nano copper oxide powder according to claim 1, wherein the preparation process comprises the following steps: the sintering temperature during the high-temperature sintering in the third step is set to be 450-550 ℃, and the sintering time is set to be 3-5 h.
9. The process for preparing nano copper oxide powder according to claim 2, wherein the purification treatment in the step III comprises the following steps: firstly, dialyzing in a distillation environment, and then carrying out rotary evaporation and freeze-drying treatment on the mixture.
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