CN108996541A - A kind of preparation method of nano zine oxide and nano-zinc oxide composite material and preparation method thereof - Google Patents
A kind of preparation method of nano zine oxide and nano-zinc oxide composite material and preparation method thereof Download PDFInfo
- Publication number
- CN108996541A CN108996541A CN201810897606.8A CN201810897606A CN108996541A CN 108996541 A CN108996541 A CN 108996541A CN 201810897606 A CN201810897606 A CN 201810897606A CN 108996541 A CN108996541 A CN 108996541A
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- China
- Prior art keywords
- nano
- zinc
- zine oxide
- nano zine
- preparation
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Links
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 41
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 276
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 138
- 239000002699 waste material Substances 0.000 claims abstract description 88
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000011701 zinc Substances 0.000 claims abstract description 49
- 238000000498 ball milling Methods 0.000 claims abstract description 46
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 46
- 238000007747 plating Methods 0.000 claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 239000000956 alloy Substances 0.000 claims abstract description 31
- 238000004512 die casting Methods 0.000 claims abstract description 31
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 150000003751 zinc Chemical class 0.000 claims abstract description 18
- 230000003287 optical effect Effects 0.000 claims abstract description 15
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 13
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 10
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 75
- 230000001376 precipitating effect Effects 0.000 claims description 58
- 239000000706 filtrate Substances 0.000 claims description 51
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 42
- 238000012545 processing Methods 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000006388 chemical passivation reaction Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 30
- 239000011248 coating agent Substances 0.000 claims description 20
- 238000000576 coating method Methods 0.000 claims description 20
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000007800 oxidant agent Substances 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 239000002932 luster Substances 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 9
- 239000008187 granular material Substances 0.000 claims description 8
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 6
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 5
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 5
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 239000008117 stearic acid Substances 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
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 3
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 159000000013 aluminium salts Chemical class 0.000 claims description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 2
- 150000001868 cobalt Chemical class 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000002161 passivation Methods 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- 229910001297 Zn alloy Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 239000011651 chromium Substances 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 18
- 239000002245 particle Substances 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 11
- 230000001954 sterilising effect Effects 0.000 abstract description 11
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 4
- 230000003712 anti-aging effect Effects 0.000 abstract description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 34
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 30
- 238000010438 heat treatment Methods 0.000 description 17
- 238000002425 crystallisation Methods 0.000 description 16
- 230000008025 crystallization Effects 0.000 description 16
- 229910021645 metal ion Inorganic materials 0.000 description 13
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical group [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 9
- 238000004821 distillation Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 229910001385 heavy metal Inorganic materials 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 239000013049 sediment Substances 0.000 description 8
- 239000002918 waste heat Substances 0.000 description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 4
- 235000011130 ammonium sulphate Nutrition 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 4
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 4
- 229940007718 zinc hydroxide Drugs 0.000 description 4
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229960001763 zinc sulfate Drugs 0.000 description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910009378 Zn Ca Inorganic materials 0.000 description 1
- AMHXQVUODFNFGR-UHFFFAOYSA-K [Ag+3].[O-]P([O-])([O-])=O Chemical group [Ag+3].[O-]P([O-])([O-])=O AMHXQVUODFNFGR-UHFFFAOYSA-K 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- WSUTUEIGSOWBJO-UHFFFAOYSA-N dizinc oxygen(2-) Chemical compound [O-2].[O-2].[Zn+2].[Zn+2] WSUTUEIGSOWBJO-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/26—Phosphorus; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/72—Organic compounds not provided for in groups B01D53/48 - B01D53/70, e.g. hydrocarbons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/244—Preparation by double decomposition of ammonium salts with sulfates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
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Abstract
The present invention relates to nano zinc oxide material technical field, specially a kind of zinc die casting alloys waste material to produce plating nickel on surface is the preparation method of the nano zine oxide of raw material and nano-zinc oxide composite material and preparation method thereof.The present invention carries out dezincification by the zinc die casting alloys waste material to plating nickel on surface and removal of impurities is handled, then it can get zinc salt by the way that alkali or ammonium bicarbonate or sodium carbonate are added into solution and controls the pH value of solution, then the uniform nano zine oxide of particle diameter distribution be made through ball milling, dehydration and sintering processes.Dispersing agent, optical components and bactericidal component are added into nano zine oxide, can get has sterilization sterilizing, removes a series of nano-zinc oxide composite materials haveing excellent performance such as formaldehyde, anti-aging.The present invention recycles zinc from waste material and prepares to form nano zine oxide and nano-zinc oxide composite material with high value, turns waste into wealth, economizes on resources, avoiding environmental pollution, and preparation is simple, preparation cost is lower.
Description
Technical field
The present invention relates to nano zinc oxide material technical field more particularly to a kind of die case zinc conjunctions to produce plating nickel on surface
Golden waste material is preparation method and nano-zinc oxide composite material of the nano zine oxide of raw material and preparation method thereof.
Background technique
Nano zine oxide (nano-ZnO) is a kind of novel high function fine inorganic product.Because the nanosizing of material, makes
It obtains nano zine oxide and produces skin effect not available for basic bulk material, small-size effect and macro quanta tunnel effect
Deng in many fields such as ceramics, chemical industry, electronics, optics, biology, medicine with important application value.
In recent years, with the rapid development of society with the continuous improvement of living standard, people are to own existence environment
Requirement also increasingly improve, therefore anti-biotic material has received widespread attention.Wherein anti-biotic material nano zine oxide causes people
Extensive concern.
Traditional high zinc zinc oxide material is widely used in the fields such as ceramics, piezoelectric transducer, catalyst and luminescent device.
Since nano zine oxide is as a kind of new function semiconductor material, compared with common zinc oxide, there is unique color
Effect, photocatalytic effect and the effect for absorbing ultraviolet light.There are many kinds of the methods for preparing nano zine oxide at present, common system
The method of standby nano zine oxide mainly has direct precipitation method, sluggish precipitation, sol-gel method, microemulsion method, hydro-thermal method, so far
Until the present, the nano zine oxide of preparation has that different degrees of reunion, degradation rate are lower.In addition, since environment is asked
Topic is got worse, and in order to protect environment, economize on resources, how to recycle zinc in environmental improvement, waste recovery use aspects, especially
It is how the Zn-Ca series in waste material feasibly to be recycled to the nano zine oxide for forming high value, is had to environment and production important
Meaning.
Summary of the invention
The present invention in view of the above-mentioned problems existing in the prior art, it is nano oxidized to obtain to provide one kind recycling zinc from waste material
The method of zinc, and what is obtained have sterilization sterilizing, go formaldehyde, the nano-zinc oxide composite material of anti-aging excellent properties and its system
Preparation Method.
To achieve the above object, the present invention uses following technical scheme.
A kind of preparation method of nano zine oxide, using the zinc die casting alloys waste material of plating nickel on surface as raw material, the waste material
There is nickel coating on surface, and nickel coating is known as nickel shell, and the preparation method comprises the steps of:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in sulfuric acid
Kirsite and nickel shell in waste material is set to be detached from and dissolve in solution, until collecting nickel shell respectively when metallic luster is presented in nickel shell surface
And solution；Then oxidant is added into solution, it is stirring while adding until being generated without precipitating；It filters and vulcanization is added into filtrate
Object, it is stirring while adding until being generated without precipitating；Followed by filtering and collect filtrate.
Preferably, the sulfuric acid solution is the dilute sulfuric acid that mass fraction is 5-12%.
Preferably, the oxidant is hydrogen peroxide, ammonium persulfate, potassium permanganate, peroxide, potassium bichromate or nitric acid.
Preferably, the sulfide is vulcanized sodium, potassium sulfide or ammonium sulfide.
S12, alkali or ammonium hydrogen carbonate or ammonium carbonate being added into filtrate, the pH value stirring while adding to filtrate is 6.5-7,
Obtain turbid solution；Then it filters and collects filtrate and precipitating respectively.
S13, the step S12 precipitating collected is placed at 140-180 DEG C dry 30-120min, obtains zinc salt；Then ball milling
Zinc salt, less than 200 μm, obtains zinc salt powder to partial size.
Preferably, in step S13, the ball milling parameter of ball milling zinc salt are as follows: revolving speed 400rad/min, Ball-milling Time 15-
100min。
S14, zinc salt powder is placed at 380-640 DEG C and heats 20-100min, obtain nano zine oxide.
Preferably, in step s 11, the nickel shell after sulfuric acid solution impregnates also is collected, and the surface of nickel shell is carried out blunt
Change processing.
The Passivation Treatment is to embathe nickel shell using chemical passivation liquid, then washes with water and removes nickel shell remained on surfaceization
Learn passivating solution.The chemical passivation liquid is the aqueous solution containing chromic acid and sulfuric acid, in every 1L chemical passivation liquid addition 8-22g chromic acid and
1-3g sulfuric acid or the chemical passivation liquid are the aqueous solutions containing potassium bichromate and glacial acetic acid, add 28- in every 1L chemical passivation liquid
55g potassium bichromate and 2-5g glacial acetic acid.
Preferably, further include that distillation processing is carried out to the step S12 filtrate collected, collect precipitate, the precipitate is
Ammonia sulfate crystal.
A kind of nano-zinc oxide composite material, including the nano zine oxide as made from approach described above, further includes: account for institute
The bactericidal component for stating nano zine oxide quality 5-20% accounts for the optical components of the nano zine oxide quality 1-10%, accounts for described
The dispersing agent of nano zine oxide quality 0.1-1.5%.
Preferably, the bactericidal component include nano silver, nano-titanium dioxide, hydroxyapatite, in diatomite at least
It is a kind of.
Preferably, the optical components include at least one of aluminium salt, cobalt salt, silver orthophosphate.
Preferably, the dispersing agent includes at least one of CTAB, PVP, calgon, stearic acid.
The preparation method of above-described nano-zinc oxide composite material, comprising the following steps:
S21, bactericidal component is added into nano zine oxide and stirs evenly, then proceed to that optical components are added and stir equal
It is even, it is subsequently added into dispersing agent and stirs evenly, obtain composite granule.
S22, so that powder is uniformly dispersed composite granule progress ball milling by dry method ball mill, it is compound to obtain nano zine oxide
Material.
Preferably, in step S22, the revolving speed of the ball milling is 250-500rad/min, Ball-milling Time 5-30min.
Preferably, in step S22, gained powder crosses the sieve of 5000 mesh after ball milling, collects sieving powder, obtains nano oxidized
Zinc composite material.
Compared with prior art, the beneficial effects of the present invention are: the present invention is useless by the zinc die casting alloys to plating nickel on surface
Material carries out dezincification and removal of impurities processing, then can be obtained by the way that alkali or ammonium bicarbonate or sodium carbonate are added into solution and controls the pH value of solution
Zinc salt is obtained, then the uniform nano zine oxide of particle diameter distribution is made through ball milling, dehydration and sintering processes.It is added into nano zine oxide
Dispersing agent, optical components and bactericidal component can get with sterilization sterilizing, go formaldehyde, anti-aging etc. are a series of to have excellent performance
Nano-zinc oxide composite material.Wherein, addition dispersing agent can prevent nano zine oxide from reuniting again, it is made to maintain nano-scale model
In enclosing, large specific surface area has effects that remove formaldehyde to improve its absorption property；Nanometer can be improved in addition optical components
The response wave band of photocatalytic activity is risen to visible region by the photocatalysis effect of zinc oxide composite；Add bactericidal component
The sterilization antibacterial effect that nano-zinc oxide composite material can be increased can be mentioned more significantly particularly by preferred bactericidal component is added
Formaldehyde performance is gone in the sterilization of high nano-zinc oxide composite material.The present invention, which recycles zinc from waste material and prepares to be formed, has high price
The nano zine oxide and nano-zinc oxide composite material of value turn waste into wealth, economize on resources, avoiding environmental pollution, and preparation process
Simple and easy, preparation cost is lower.In addition, also can be used as the high-purity sulfuric acid that chemical fertilizer utilizes by the method for the invention
Ammonium, while the other impurity (metal impurities contained by waste material) having been dissolved in solution can be settled out from solution in treatment process
It recycles, thus so that the method for the present invention will not be generated waste discharge in production and is caused secondary pollution, the method for the present invention green
Environmental protection.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph after nano zine oxide prepared by embodiment 1 is placed one month；
Fig. 2 is the grain size distribution after nano zine oxide prepared by embodiment 7 is placed one month；
Fig. 3 is the scanning electron microscope (SEM) photograph after nano zine oxide prepared by embodiment 8 is placed one month.
Specific embodiment
In order to more fully understand technology contents of the invention, combined with specific embodiments below to technical solution of the present invention
It is described further and illustrates.
Embodiment 1
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: being added oxidant (hydrogen peroxide) in solution, stirring while adding until generating without precipitating；Solution
In in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as Cu2+、Ni2+、Cd2+、Mn2+、
Pb2+Equal metal ions.It filters and is added into solution sulfide (ammonium sulfide solution that mass percent is 10%), side edged stirs
It mixes until being generated without precipitating；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、Cd2+、Mn2+、Pb2+Equal gold
Belong to ion and generate corresponding sediment CuS, NiS, CdS, MnS, PbS, avoids the harm of Heavy-metal Polluted Environment, cause secondary
Pollution.
Processing to the nickel shell pulled out: being passivated processing to the surface of nickel shell, specifically embathes nickel shell 5- with passivating solution
10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell passivating solution remained on surface.
The chemical passivation liquid is the aqueous solution containing chromic acid and sulfuric acid, in every 1L chemical passivation liquid addition 8-22g chromic acid and
1-3g sulfuric acid.
S12, ammonium hydrogen carbonate is added into filtrate, the pH stirring while adding to filtrate is 6.8, obtains whole basic carbonates
Zinc and ammonium sulfate；Then it filters and collects filtrate and precipitating respectively, be precipitated as the basic zinc carbonate with the crystallization water, precipitating is in
White.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling zinc salt obtains basic zinc carbonate powder to partial size less than 200 μm.Ball milling parameter are as follows:
Revolving speed is 400rad/min, Ball-milling Time 100min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace is sintered, temperature is 550 DEG C, and heating time is
100min obtains nano zine oxide.For the partial size of gained nano zine oxide within the scope of 15-25nm, particle diameter distribution is uniform.
Embodiment 2
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 6% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: oxidant (liquor potassic permanganate that mass percent is 34%), side edged are added in solution
Stirring without precipitating until generate；In solution in addition to having dissolved the zinc in waste material, also dissolved with other foreign metals member in waste material
Element, such as Cu2+、Ni2+、Cd2+、Mn2+、Pb2+Equal metal ions.
Then it is added into solution sulfide (ammonium sulfide solution that mass percent is 40%), it is stirring while adding until nothing
Precipitating generates；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、 Cd2+、Mn2+、Pb2+Equal metal ions
Corresponding sediment CuS, NiS, CdS, MnS, PbS are generated, the harm of Heavy-metal Polluted Environment is avoided, causes secondary pollution.
Processing to the nickel shell pulled out: being passivated processing to the surface of nickel shell, specifically embathes nickel shell 5- with passivating solution
10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell passivating solution remained on surface.
The chemical passivation liquid is the aqueous solution containing potassium bichromate and glacial acetic acid, adds 28-55g in every 1L chemical passivation liquid
Potassium bichromate and 2-5g glacial acetic acid.
S12, be added ammonium carbonate into filtrate, the pH stirring while adding to filtrate is 7, obtain whole basic zinc carbonate and
Ammonium sulfate；Then it filters and collects filtrate and precipitating respectively, be precipitated as the basic zinc carbonate with the crystallization water, precipitating is in white
Color.
S13, the step S12 precipitating collected is placed at 180 DEG C dry 30min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling zinc salt obtains basic zinc carbonate powder to partial size less than 200 μm.Ball milling parameter are as follows:
Revolving speed is 400rad/min, Ball-milling Time 15min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace is sintered, temperature is 640 DEG C, and heating time is
30min obtains nano zine oxide.For the partial size of gained nano zine oxide within the scope of 20-30nm, particle diameter distribution is uniform.
Embodiment 3
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: being added oxidant (ammonium persulfate that mass percent is 30%) in solution, stirring while adding
Until being generated without precipitating；In solution in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as
Cu2+、Ni2+、Cd2+、Mn2+、Pb2+Equal metal ions.
Then it is added into solution sulfide (potassium sulfide solution that mass percent is 10%), it is stirring while adding until nothing
Precipitating generates；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、 Cd2+、Mn2+、Pb2+Equal metal ions
Corresponding sediment CuS, NiS, CdS, MnS, PbS are generated, the harm of Heavy-metal Polluted Environment is avoided, causes secondary pollution.
Processing to the nickel shell pulled out: processing is passivated to the surface of nickel shell, specifically embathes nickel with chemical passivation liquid
Shell 5-10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell chemical passivation liquid remained on surface.It uses
Chemical passivation liquid it is identical as embodiment 1.
S12, ammonium hydrogen carbonate is added into filtrate, the pH stirring while adding to filtrate is 6.5, obtains whole basic carbonates
Zinc and ammonium sulfate；Then it filters and collects filtrate and precipitating respectively, be precipitated as the basic zinc carbonate with the crystallization water, precipitating is in
White.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling zinc salt obtains basic zinc carbonate powder to partial size less than 200 μm.Ball milling parameter are as follows:
Revolving speed is 400rad/min, Ball-milling Time 100min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace is sintered, temperature is 500 DEG C, and heating time is
80min obtains nano zine oxide.For the partial size of gained nano zine oxide within the scope of 20-30nm, particle diameter distribution is uniform.
Embodiment 4
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: being added oxidant (hydrogen peroxide) in solution, stirring while adding until generating without precipitating；Solution
In in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as Cu2+、Ni2+、Cd2+、Mn2+、
Pb2+Equal metal ions.Then sulfide (sodium sulfide solution that mass percent is 10%) is added into solution, side edged stirs
It mixes until being generated without precipitating；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、Cd2+、Mn2+、Pb2+Equal gold
Belong to ion and generate corresponding sediment CuS, NiS, CdS, MnS, PbS, avoids the harm of Heavy-metal Polluted Environment, cause secondary
Pollution.
Processing to the nickel shell pulled out: processing is passivated to the surface of nickel shell, specifically embathes nickel with chemical passivation liquid
Shell 5-10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell chemical passivation liquid remained on surface.It uses
Chemical passivation liquid it is identical as embodiment 1.
S12, ammonium hydroxide is added into filtrate, the pH stirring while adding to filtrate is 6.8, obtains turbid solution；Then it filters simultaneously
Filtrate and precipitating are collected respectively, is precipitated as the zinc hydroxide with the crystallization water, are precipitated white.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains zinc hydroxide；Then partial size is milled to less than 200 μm, obtains zinc hydroxide powder.Ball milling parameter are as follows: revolving speed is
400rad/min, Ball-milling Time 100min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it zinc hydroxide powder is placed in Muffle furnace is sintered, temperature is 500 DEG C, and heating time 90min is obtained
To nano zine oxide.For the partial size of gained nano zine oxide within the scope of 20-30nm, particle diameter distribution is uniform.
Embodiment 5
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: being added oxidant (hydrogen peroxide) in solution, stirring while adding until generating without precipitating；Solution
In in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as Cu2+、Ni2+、Cd2+、Mn2+、
Pb2+Equal metal ions.Then sulfide (sodium sulfide solution that mass percent is 10%) is added into solution, side edged stirs
It mixes until being generated without precipitating；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、Cd2+、Mn2+、Pb2+Equal gold
Belong to ion and generate corresponding sediment CuS, NiS, CdS, MnS, PbS, avoids the harm of Heavy-metal Polluted Environment, cause secondary
Pollution.
Processing to the nickel shell pulled out: processing is passivated to the surface of nickel shell, specifically embathes nickel with chemical passivation liquid
Shell 5-10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell chemical passivation liquid remained on surface.It uses
Chemical passivation liquid it is identical as embodiment 1.
S12, ammonium hydrogen carbonate is added into filtrate, the pH stirring while adding to filtrate is 6.1, obtains turbid solution；Then it crosses
Filtrate and precipitating are filtered and collect respectively, precipitating is mainly the basic zinc carbonate with the crystallization water, and precipitating is in light brown, is had in precipitating miscellaneous
Matter.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling zinc salt obtains basic zinc carbonate powder to partial size less than 200 μm.Ball milling parameter are as follows:
Revolving speed is 400rad/min, Ball-milling Time 100min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace is sintered, temperature is 500 DEG C, and heating time is
100min obtains nano zine oxide.For the partial size of gained nano zine oxide within the scope of 50-60nm, particle diameter distribution is uniform.
Embodiment 6
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: being added oxidant (hydrogen peroxide) in solution, stirring while adding until generating without precipitating；Solution
In in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as Cu2+、Ni2+、Cd2+、Mn2+、
Pb2+Equal metal ions.
Then it is added into solution sulfide (sodium sulfide solution that mass percent is 10%), it is stirring while adding until nothing
Precipitating generates；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、 Cd2+、Mn2+、Pb2+Equal metal ions
Corresponding sediment CuS, NiS, CdS, MnS, PbS are generated, the harm of Heavy-metal Polluted Environment is avoided, causes secondary pollution.
Processing to the nickel shell pulled out: processing is passivated to the surface of nickel shell, specifically embathes nickel with chemical passivation liquid
Shell 5-10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell chemical passivation liquid remained on surface.It uses
Chemical passivation liquid it is identical as embodiment 1.
S12, ammonium hydrogen carbonate is added into filtrate, the pH stirring while adding to filtrate is 7.3, obtains turbid solution；Then it crosses
Filtrate and precipitating are filtered and collect respectively, precipitating is mainly the basic zinc carbonate with the crystallization water, and precipitating is in light brown, is had in precipitating miscellaneous
Matter.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling zinc salt obtains basic zinc carbonate powder to partial size less than 200 μm.Ball milling parameter are as follows:
Revolving speed is 400rad/min, Ball-milling Time 100min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace being sintered, temperature is 500 DEG C, heating time 90min,
Obtain nano zine oxide.For the partial size of gained nano zine oxide within the scope of 50-60nm, particle diameter distribution is uniform.
Embodiment 7
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% makes kirsite and nickel shell in waste material be detached from and dissolve, and metallic luster is presented in nickel shell surface
When, it pulls nickel shell out, collects solution.
Processing to solution: being added oxidant (hydrogen peroxide) in solution, stirring while adding until generating without precipitating；Solution
In in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as Cu2+、Ni2+、Cd2+、Mn2+、
Pb2+Equal metal ions.
Then it is added into solution sulfide (sodium sulfide solution that mass percent is 10%), it is stirring while adding until nothing
Precipitating generates；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、 Cd2+、Mn2+、Pb2+Equal metal ions
Corresponding sediment CuS, NiS, CdS, MnS, PbS are generated, the harm of Heavy-metal Polluted Environment is avoided, causes secondary pollution.
Processing to the nickel shell pulled out: processing is passivated to the surface of nickel shell, specifically embathes nickel with chemical passivation liquid
Shell 5-10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell chemical passivation liquid remained on surface.It uses
Chemical passivation liquid it is identical as embodiment 1.
S12, ammonium hydrogen carbonate is added into filtrate, the pH stirring while adding to filtrate is 6.8, obtains turbid solution；Then it crosses
It filters and collects filtrate and precipitating respectively, be precipitated as the basic zinc carbonate with the crystallization water, precipitate white.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling basic zinc carbonate obtains basic zinc carbonate powder to partial size at 350-500 μm.Ball
Grind parameter are as follows: revolving speed 400rad/min, Ball-milling Time 7min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace being sintered, temperature is 500 DEG C, heating time 80min,
Obtain nano zine oxide.The D of gained nano zine oxideV(50) partial size is 30nm, is existed at 0.2-1 μm and 10-200 μm certain
Distribution, particle diameter distribution is wider, compared to embodiment 1-4 preparation nano zine oxide, this implementations prepare nano zine oxide grain
Diameter is unevenly distributed.
Embodiment 8
The present embodiment provides a kind of preparation methods of nano zine oxide, are original with the zinc die casting alloys waste material of plating nickel on surface
Material, zinc die casting alloys are the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and specific steps are such as
Under:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in quality
12h in the dilute sulfuric acid that score is 12% collects solution until pulling nickel shell out when metallic luster is presented in nickel shell surface.
Processing to solution: being added oxidant (hydrogen peroxide) in solution, stirring while adding until generating without precipitating；Solution
In in addition to having dissolved the zinc in waste material, also dissolved with other impurity metallic elements in waste material, such as Cu2+、Ni2+、Cd2+、Mn2+、
Pb2+Equal metal ions.
Then it is added into solution sulfide (ammonium sulfide solution that mass percent is 10%), it is stirring while adding until nothing
Precipitating generates；Followed by filtering and collect filtrate.Sulfide is added can be by Cu2+、Ni2+、 Cd2+、Mn2+、Pb2+Equal metal ions
Corresponding sediment CuS, NiS, CdS, MnS, PbS are generated, the harm of Heavy-metal Polluted Environment is avoided, causes secondary pollution.
Processing to the nickel shell pulled out: processing is passivated to the surface of nickel shell, specifically embathes nickel with chemical passivation liquid
Shell 5-10s makes nickel shell surface form dense oxidation film, then washes with water and removes nickel shell passivating solution remained on surface.The change used
It is identical as embodiment 1 to learn passivating solution.
S12, ammonium hydrogen carbonate is added into filtrate, the pH stirring while adding to filtrate is 6.8, obtains whole basic carbonates
Zinc and ammonium sulfate；Then it filters and collects filtrate and precipitating respectively, be precipitated as the basic zinc carbonate with the crystallization water, precipitating is in
White.
S13, the step S12 precipitating collected is placed at 140 DEG C dry 120min, removes the Free water and crystallization in precipitating
Water obtains basic zinc carbonate；Then ball milling zinc salt obtains basic zinc carbonate powder to partial size less than 200 μm.Ball milling parameter are as follows:
Revolving speed is 400rad/min, Ball-milling Time 100min.
The filtrate that step S12 is collected carries out distillation processing, is evaporated to when only remaining a small amount of residual moisture, stops heating, by
Remaining a small amount of moisture is evaporated by waste heat, recycles crystal, crystal is ammonia sulfate crystal.
S14, it basic zinc carbonate powder is placed in Muffle furnace is sintered, temperature is 750 DEG C, and heating time is
100min obtains nano zine oxide.The partial size of gained nano zine oxide occurs reuniting existing within the scope of 25-50nm, between crystal grain
As comparing embodiment 1-4, heat treatment temperature increases, and crystal continued growth, crystal form is gradually perfect, and crystallite dimension becomes larger, while brilliant
Also start agglomeration occur between grain.
Embodiment 9
The present embodiment provides the preparation sides of a kind of nano-zinc oxide composite material and this kind of nano-zinc oxide composite material
Method.
Nano-zinc oxide composite material is made of nano zine oxide, bactericidal component, optical components, dispersing agent.
Bactericidal component accounts for the 10% of nano zine oxide weight: by etc. quality partial size be 30-50nm nano silver, partial size is
Nano-titanium dioxide, hydroxyapatite, the diatomite composition of 50-70nm.
Optical components account for the 10% of nano zine oxide weight: by etc. quality aluminum nitrate, cobalt nitrate (Co2+), silver orthophosphate group
At.
Dispersing agent accounts for the 1.5% of nano zine oxide weight: by etc. PVP, calgon, the stearic acid of quality form.
Specific step is as follows:
Bactericidal component is added nano zine oxide prepared by S21, Example 1 into nano zine oxide and stirs evenly, so
After continuously add optical components and stir evenly, be subsequently added into dispersing agent and stir evenly, obtain composite granule.
S22, powder is made to be uniformly dispersed composite granule progress ball milling by dry method ball mill, gained powder mistake after ball milling
The sieve of 5000 mesh collects sieving powder, obtains nano-zinc oxide composite material.The parameter of dry ball milling are as follows: revolving speed 500rad/
Min, Ball-milling Time 5min.
Embodiment 10
The present embodiment provides the preparation sides of a kind of nano-zinc oxide composite material and this kind of nano-zinc oxide composite material
Method.
Nano-zinc oxide composite material is made of nano zine oxide, bactericidal component, optical components, dispersing agent.
Bactericidal component is the nano-titanium dioxide that partial size is 50-70nm, accounts for the 5% of nano zine oxide weight；Optical components
For silver orthophosphate, the 1% of nano zine oxide weight is accounted for；Dispersing agent is CTAB, accounts for the 0.5% of nano zine oxide weight.
Specific step is as follows:
Bactericidal component is added nano zine oxide prepared by S21, Example 1 into nano zine oxide and stirs evenly, so
After continuously add optical components and stir evenly, be subsequently added into dispersing agent and stir evenly, obtain composite granule.
S22, powder is made to be uniformly dispersed composite granule progress ball milling by dry method ball mill, gained powder mistake after ball milling
The sieve of 5000 mesh collects sieving powder, obtains nano-zinc oxide composite material.The parameter of dry ball milling are as follows: revolving speed 250rad/
Min, Ball-milling Time 30min.
Embodiment 11-17
Embodiment 11-17 provides a kind of nano-zinc oxide composite material and preparation method.It is received used in each embodiment
Rice crude zinc oxide materials are different from embodiment 9 outer, and the raw materials and consumption that other components use is consistent with embodiment 9, and prepare
Method is also consistent with embodiment 9.The nano zine oxide raw material difference that embodiment 11-17 is used is as shown in table 1 below.
The nano zine oxide that 1 embodiment 11-17 of table is used
| Embodiment | Nano zine oxide |
| 11 | Nano zine oxide prepared by embodiment 2 |
| 12 | Nano zine oxide prepared by embodiment 3 |
| 13 | Nano zine oxide prepared by embodiment 4 |
| 14 | Nano zine oxide prepared by embodiment 5 |
| 15 | Nano zine oxide prepared by embodiment 6 |
| 16 | Nano zine oxide prepared by embodiment 7 |
| 17 | Nano zine oxide prepared by embodiment 8 |
Embodiment 18
The present embodiment provides the preparation sides of a kind of nano-zinc oxide composite material and this kind of nano-zinc oxide composite material
Method.The dosage of the used bactericidal component of the present embodiment and dispersing agent is different from embodiment 9 outer, raw material that other components use and
Dosage is consistent with embodiment 9, and preparation method is also consistent with embodiment 9.
The dosage of the used bactericidal component of the present embodiment and dispersing agent is as follows:
Bactericidal component accounts for the 20% of nano zine oxide weight: by etc. quality partial size be 30-50nm nano silver, partial size is
Nano-titanium dioxide, hydroxyapatite, the diatomite composition of 50-70nm.
Dispersing agent accounts for the 0.1% of nano zine oxide weight: by etc. PVP, calgon, the stearic acid of quality form.
Embodiment 19-20
Embodiment 19-20 provides a kind of nano-zinc oxide composite material and preparation method.It is killed used in each embodiment
Bacterium component is different from embodiment 9 outer, and the raw materials and consumption that other components use is consistent with embodiment 9, and preparation method
It is consistent with embodiment 9.The nano zine oxide raw material difference that embodiment 19-20 is used is as shown in table 2 below.
The bactericidal component that 2 embodiment 19-20 of table is used
| Embodiment | Bactericidal component |
| 19 | Partial size is the nano-titanium dioxide of 130-150nm |
| 20 | Partial size is the nano zine oxide of 130-150nm |
Test one: the bactericidal property of the nano-zinc oxide composite material of detection embodiment 9-20 preparation
Detection method is as follows:
Test method:
The nano-zinc oxide composite material aqueous solution that configuration quality percentage is 1.5%, is dispersed with ultrasonic wave, is sample
Liquid.
Sample liquid is uniformly mixed in equal volume with staphylococcus aureus liquid, then shakes 30min on the oscillator, then
It takes on the solution even spread to experiment plate of 50mL, by compareing for the experiment plate and non-plus nano zinc oxide composite
Plate is put into thermostatic chamber together, and placement is taken out for 24 hours, then its clump count of number calculates sterilizing rate.
Sterilizing rate=(clump count-sample experiments clump count of control experiment)/control experiment clump count × 100% inspection
It is as shown in table 3 below to survey result.
Sterilizing rate of the nano-zinc oxide composite material of 3 embodiment 9-19 of table preparation to staphylococcus aureus
Test two: the reunion situation of the nano-zinc oxide composite material of detection embodiment 9-17 preparation
Detection method is as follows: it is 1.5cm, the sample of a height of 3cm that the embodiment 1-8 nano zine oxide prepared, which is contained in diameter,
It places 1 month in product bottle, then observes the nano zine oxide of each embodiment preparation respectively with scanning electron microscope and particle diameter distribution instrument
Reunion situation and particle diameter distribution situation.The scanning electron microscope (SEM) photograph and grain size distribution that embodiment 1,7,8 prepares nano zine oxide are as schemed
1, shown in Fig. 2 and Fig. 3, observation result is as follows:
Embodiment 1: from the figure, it can be seen that gained crystal grain distribution is uniform, very fine and close between crystal grain, average grain size
In 18nm or so, agglomeration is seldom observed.
Embodiment 7: from the figure, it can be seen that the D of gained nano zine oxideV(50) partial size be 30nm, at 0.2-1 μm and
10-200 μm there are certain distribution, particle diameter distribution is wider, compares embodiment 1-4, particle diameter distribution is uneven.
Embodiment 8: from the figure, it can be seen that the partial size of gained nano zine oxide within the scope of 25-50nm, goes out between crystal grain
Existing agglomeration compares embodiment 1-4, and sintering temperature increases, and crystal continued growth, crystal form is gradually perfect, and crystallite dimension becomes larger,
Also start agglomeration occur between crystal grain simultaneously.
It is described above that technology contents of the invention are only further illustrated with embodiment, in order to which reader is easier to understand,
But embodiments of the present invention are not represented and are only limitted to this, any technology done according to the present invention extends or recreation, is sent out by this
Bright protection.
Claims (12)
1. a kind of preparation method of nano zine oxide, which is characterized in that using the zinc die casting alloys waste material of plating nickel on surface as raw material, pressure
Cast zinc alloy is the casting of plating nickel on surface, i.e. there is nickel coating on the surface of waste material, and nickel coating is known as nickel shell, and the preparation method includes
Following steps:
S11, crusher surface nickel plating first zinc die casting alloys waste material, obtain broken waste material；Waste material is soaked in sulfuric acid solution
In be detached from kirsite in waste material and nickel shell and dissolve, until when metallic luster is presented in nickel shell surface, collect nickel shell and molten respectively
Liquid；Then oxidant is added into solution, it is stirring while adding until being generated without precipitating；Sulfide is filtered and is added into filtrate,
It is stirring while adding to be generated up to without precipitating；Followed by filtering and collect filtrate；
S12, alkali or ammonium hydrogen carbonate or ammonium carbonate are added into filtrate, the pH value stirring while adding to filtrate is 6.5-7, is obtained muddy
Turbid；Then it filters and collects filtrate and precipitating respectively；
S13, the step S12 precipitating collected is placed at 140-180 DEG C dry 30-120min, obtains zinc salt；Then ball milling zinc salt
To partial size less than 200 μm, zinc salt powder is obtained；
S14, zinc salt powder is placed at 380-640 DEG C and heats 20-100min, obtain nano zine oxide.
2. the preparation method of nano zine oxide according to claim 1, which is characterized in that in step S11, the oxidant is
Hydrogen peroxide, ammonium persulfate, potassium permanganate, peroxide, potassium bichromate or nitric acid.
3. the preparation method of nano zine oxide according to claim 1, which is characterized in that in step S11, the sulfide is
Vulcanized sodium, potassium sulfide or ammonium sulfide.
4. the preparation method of nano zine oxide according to claim 1, which is characterized in that in step S13, the ball of ball milling zinc salt
Grind parameter are as follows: revolving speed 400rad/min, Ball-milling Time 15-100min.
5. the preparation method of nano zine oxide according to claim 1, which is characterized in that also collected through sulfuric acid in step S11
Nickel shell after solution immersion, and processing is passivated to the surface of nickel shell.
6. the preparation method of nano zine oxide according to claim 5, which is characterized in that the Passivation Treatment is using chemistry
Passivating solution embathes waste material, then washes with water and removes the remaining chemical passivation liquid of scraped surface；The chemical passivation liquid is containing chromium
The aqueous solution of acid and sulfuric acid adds 8-22g chromic acid and 1-3g sulfuric acid in every 1L chemical passivation liquid or the chemical passivation liquid is to contain
The aqueous solution of potassium bichromate and glacial acetic acid adds 28-55g potassium bichromate and 2-5g glacial acetic acid in every 1L chemical passivation liquid.
7. a kind of nano-zinc oxide composite material, which is characterized in that including the nano zine oxide prepared by claim 1, also wrap
It includes: accounting for the bactericidal component of the nano zine oxide quality 5-20%, account for the optical components of the nano zine oxide quality 1-10%,
Account for the dispersing agent of the nano zine oxide quality 0.1-1.5%.
8. nano-zinc oxide composite material according to claim 7, which is characterized in that the bactericidal component includes nanometer
At least one of silver, nano-titanium dioxide, hydroxyapatite, diatomite.
9. nano-zinc oxide composite material according to claim 7, which is characterized in that the optical components include aluminium salt,
At least one of cobalt salt, silver orthophosphate.
10. nano-zinc oxide composite material according to claim 7, which is characterized in that the dispersing agent include CTAB,
At least one of PVP, calgon, stearic acid.
11. a kind of preparation method of nano-zinc oxide composite material as claimed in claim 7, which is characterized in that including following step
It is rapid:
S21, bactericidal component is added into nano zine oxide and stirs evenly, then proceed to that optical components are added and stir evenly,
It is subsequently added into dispersing agent and stirs evenly, obtain composite granule；
S22, so that powder is uniformly dispersed composite granule progress ball milling by dry method ball mill, obtain nano zine oxide composite wood
Material.
12. the preparation method of nano-zinc oxide composite material according to claim 11, which is characterized in that in step S22, institute
The revolving speed for stating ball milling is 250-500rad/min, Ball-milling Time 5-30min.
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Application publication date: 20181214 Assignee: Zhongxing (Guangzhou) nano materials Co.,Ltd. Assignor: Shen Haihong Contract record no.: X2020440000126 Denomination of invention: The invention relates to a preparation method of nano zinc oxide, nano zinc oxide composite material and preparation method thereof Granted publication date: 20200901 License type: Exclusive License Record date: 20201014 |