CN109276474A - A kind of preparation method of nano zine oxide/cationic polysaccharide hybrid nanomaterial - Google Patents
A kind of preparation method of nano zine oxide/cationic polysaccharide hybrid nanomaterial Download PDFInfo
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- CN109276474A CN109276474A CN201811157702.5A CN201811157702A CN109276474A CN 109276474 A CN109276474 A CN 109276474A CN 201811157702 A CN201811157702 A CN 201811157702A CN 109276474 A CN109276474 A CN 109276474A
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- China
- Prior art keywords
- cationic polysaccharide
- nano zine
- zine oxide
- solution
- hybrid nanomaterial
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- -1 cationic polysaccharide Chemical class 0.000 title claims abstract description 49
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 34
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 34
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000011787 zinc oxide Substances 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 19
- 239000002537 cosmetic Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 235000013339 cereals Nutrition 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 230000010494 opalescence Effects 0.000 claims description 6
- 239000006071 cream Substances 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 22
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 238000012216 screening Methods 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 28
- 229920001661 Chitosan Polymers 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000002835 absorbance Methods 0.000 description 12
- 239000004201 L-cysteine Substances 0.000 description 11
- 150000003254 radicals Chemical class 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 10
- 235000013878 L-cysteine Nutrition 0.000 description 10
- 239000000523 sample Substances 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 235000019198 oils Nutrition 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 4
- 235000006708 antioxidants Nutrition 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- 230000002000 scavenging effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 3
- 239000000516 sunscreening agent Substances 0.000 description 3
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical group 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- UREZNYTWGJKWBI-UHFFFAOYSA-M benzethonium chloride Chemical compound [Cl-].C1=CC(C(C)(C)CC(C)(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 UREZNYTWGJKWBI-UHFFFAOYSA-M 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000008390 olive oil Nutrition 0.000 description 2
- 239000004006 olive oil Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 108090000765 processed proteins & peptides Proteins 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 235000013904 zinc acetate Nutrition 0.000 description 2
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 description 1
- OJIBJRXMHVZPLV-UHFFFAOYSA-N 2-methylpropyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCC(C)C OJIBJRXMHVZPLV-UHFFFAOYSA-N 0.000 description 1
- 238000004483 ATR-FTIR spectroscopy Methods 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229920002907 Guar gum Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- DIWNCNINVWYUCD-UHFFFAOYSA-N acetyl acetate;zinc Chemical compound [Zn].CC(=O)OC(C)=O DIWNCNINVWYUCD-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006701 autoxidation reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000008366 buffered solution Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- HEILIGJNYTWOHU-UHFFFAOYSA-N ethanol 2-hydroxybenzoic acid Chemical compound CCO.OC(=O)C1=CC=CC=C1O HEILIGJNYTWOHU-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical group 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 210000001541 thymus gland Anatomy 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- BEAZKUGSCHFXIQ-UHFFFAOYSA-L zinc;diacetate;dihydrate Chemical compound O.O.[Zn+2].CC([O-])=O.CC([O-])=O BEAZKUGSCHFXIQ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/025—Explicitly spheroidal or spherical shape
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/27—Zinc; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
- A61K8/447—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof containing sulfur
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/737—Galactomannans, e.g. guar; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Dermatology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of nano zine oxide/cationic polysaccharide hybrid nanomaterials and preparation method thereof, belong to composite nanometer particle technical field.A kind of nano zine oxide/cationic polysaccharide hybrid nanomaterial is prepared by cationic polysaccharide/containing mercaptoamino acid/nanometer zinc oxide precursor mixed solution in the present invention, and preparation method is simple, and cost is relatively low.Hybrid nanomaterial of the present invention has preferable dispersibility, photostability compared with existing granular materials, in addition to this lower photocatalytic activity also has preferable inoxidizability and emulsifiability, can be used in sunlight screening skin-protecting product and other anti-ultraviolet materials.
Description
Technical field
The present invention relates to a kind of nano zine oxide/cationic polysaccharide hybrid nanomaterials and preparation method thereof, belong to compound
Field of nanoparticles.
Background technique
Inorganic sunscreen is that the physical sunscreen of anti-sunlight function is played and a kind of reflection by ultraviolet light, refraction and scattering
Agent, when its partial size is in 1-100nm, then referred to as inorganic nano sunlight screening agent.Inorganic nano sunlight screening agent and common inorganic sun-screening agent phase
Than partial size is small, large specific surface area, can absorb ultraviolet light, can also reflect ultraviolet light, has stronger barrier energy to ultraviolet light
Power.However, because its partial size is small, there are large specific surface area, lead to that its is easy to reunite, photocatalytic activity is high, easy skin permeation gives people
Health cause it is potentially hazardous.The problems such as its is easy to reunite, photocatalytic activity is high in order to solve, easy skin permeation, currently, main
It takes surface to cover coating method, such as is coated using aluminium oxide, fatty acid, dimethyl polysiloxane, natural macromolecular etc.
Titanium dioxide granule makes it: it is 1. surface inerting, improve the progress of its photochemical stability；2. increasing its partial size after cladding, reduce
Its percutaneous permeability；3. surface has different functional groups, can be well dispersed in by the titanium dioxide of surface treatment
In different media.
For example, [Xiao J, Chen W, Wang F, the et al.Polymer/TiO2Hybrid such as Xiao Jie
Nanoparticles with Highly Effective UV-Screening but Eliminated
Photocatalytic Activity [J] .Macromolecules, 2013,46 (2): 375-383.] by triblock polymer
PEO-b-PDMA-b-PS carries out the colloidal particle that self assembly preparation has core-shell structure in THF/EtOH, then by nano-silica
The presoma tetraethyl titanate for changing titanium is added in micellar solution, is prepared for polymer/TiO2 hydridization by sol gel reaction
Colloidal particle has preferable dispersibility, low photocatalytic activity and preferable sun-proof performance.In the recent period, Anna Regiel etc.
[Regielfutyra A,M,S,et al.The quenching effect of chitosan
crosslinking on ZnO nanoparticles photocatalytic activity[J].Rsc Advances,
2015,5 (97): 80089-80097.] it reports by adding crosslinking agent trimerization phosphorus for chitosan and nano zine oxide blending
Sour sodium makes chitosan crosslinked in surface of nanometer zinc oxide, to improve the dispersibility of nano zine oxide, and its photochemical activity is quenched.
However, the current resulting grain diameter of method times is so relatively large, dispersibility is poor, and there is no obtain for photocatalytic activity
To significant inhibiting effect, and then constrain the development of nano sunlight screening agent.
Summary of the invention
In order to overcome bad dispersibility existing for above-mentioned nano zine oxide in the prior art, photocatalytic activity high and easily infiltration
The problem of into skin, the present invention probes into nano zinc oxide modified method, by cationic polysaccharide/L-cysteine/
A kind of nano zine oxide/cationic polysaccharide hybrid nanomaterial, gained one is prepared in nanometer zinc oxide precursor mixed solution
Kind nano zine oxide/cationic polysaccharide hybrid nanomaterial good dispersion, photocatalytic activity are low low with percutaneous permeability, are a kind of
With sun-proof and anti-oxidation function hybridized nanometer sunblock particles.
There is provided a kind of nano zine oxide/cationic polysaccharide hybrid nanomaterial preparation sides for first purpose of the invention
Method, the preparation method include:
(1) cationic polysaccharide solution and the mixing of acid solution containing sulfhydryl amino, are added nanometer zinc oxide precursor, stir at room temperature
Mix for 24 hours until nanometer zinc oxide precursor be completely dissolved, obtain cationic polysaccharide/L-cysteine/nanometer zinc oxide precursor
Mixed solution；
(2) aqueous alkali is added to above-mentioned mixed solution and adjusts mixed solution pH to 7, solution shows blue opalescence, obtains
Hybrid nanomaterial.
In one embodiment of the invention, the cationic polysaccharide is with the mass concentration ratio containing mercaptoamino acid
(0.5~6): 1.
In one embodiment of the invention, the nanometer zinc oxide precursor with containing mercaptoamino acid and quality it is dense
Degree is than being (0.1~6): 1.
In one embodiment of the invention, the nano zine oxide/cationic polysaccharide hybrid nanomaterial preparation
Method prepares aqueous acid containing sulfhydryl amino, by bodies such as the two specifically includes the following steps: preparing cationic polysaccharide aqueous solution
Long-pending mixing, is added nanometer zinc oxide precursor, stirs at room temperature for 24 hours until it is completely dissolved, then is adjusted and mixed with alkaline conditioner
Closing pH value of solution is 5~8, and colourless solution shows blue opalescence, obtains nano zine oxide/cationic polysaccharide hybrid nanomaterial；
In terms of weight fraction, each reactant dosage formula is as follows:
10~200 parts of cationic polysaccharide,
Containing 20~100 parts of mercaptoamino acid,
50~200 parts of nanometer zinc oxide precursor.
In one embodiment of the invention, in the mixed solution nanometer zinc oxide precursor be acetic anhydride zinc,
One of Zinc diacetate dihydrate, six hydration zinc acetates, zinc carbonate or a variety of mixtures.
In one embodiment of the invention, the concentration of the nanometer zinc oxide precursor is 0.5~10mg/mL.
In one embodiment of the invention, the nanometer zinc oxide precursor preferentially selects zinc acetate, concentration 5
~10mg/mL.
In one embodiment of the invention, described containing mercaptoamino acid includes L-cysteine or by sulfhydrylation
Learn the amino acid of modification.
In one embodiment of the invention, the cationic polysaccharide include n-trimethyl chitosan chloride, cationization it is transparent
One of matter acid, cation guar gum, cationic cellulose or a variety of mixtures.
In one embodiment of the invention, the cationic polysaccharide solution is 1~6mg/mL aqueous solution.
In one embodiment of the invention, the acid solution containing sulfhydryl amino is 2~4mg/mL aqueous solution.
In one embodiment of the invention, the volume ratio of the cationic polysaccharide solution and the acid solution containing sulfhydryl amino
For 1:(1-1.5).
In one embodiment of the invention, the alkaline conditioner preferentially selects NaOH aqueous solution, and concentration is
0.4-0.6M。
The nano zine oxide being prepared a second object of the present invention is to provide the method/cationic polysaccharide hydridization is received
Rice grain.
Third object of the present invention is to provide a kind of cosmetic product, the cosmetic product is comprising described in claim 8
Nano zine oxide/cationic polysaccharide hybrid nanomaterial.
In one embodiment of the invention, the cosmetic product includes greasepaint or lotion or cream.
It is sun-proof in cosmetics that fourth object of the present invention is to provide nano zine oxide/cationic polysaccharide hybrid nanomaterial
Or the application in other uvioresistant absorbing material fields.
Beneficial effect of the present invention
The present invention prepare the raw materials used cationic polysaccharide of hybrid nanomaterial and containing mercaptoamino acid it is cheap and easy to get, have compared with
Good biocompatibility, preparation process is simple and convenient, and cationic polysaccharide has the function of radicals scavenging, assigns hybridized nanometer
Grain antioxygenic property, can be used for Skin whitening care cosmetics well.The present invention solves nano zine oxide since partial size is easy to reunite, dispersion
Property difference problem cationic polysaccharide and nano zine oxide is wrapped up containing mercaptoamino acid in self assembling process, also solve it
It easily permeates, photostability is poor, having the problem of photocatalytic activity, it can effective shield ultraviolet radiation simultaneously.Present invention preparation
Hybrid particulates all there is preferable emulsifiability to different cosmetics oils, may act as emulsifying in the preparation of lotion cream etc.
Agent uses.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of hydridization colloidal particle prepared by the present invention；
Fig. 2 is that the TEM and SEM of hydridization colloidal particle prepared by the present invention scheme, wherein (A1), (B1) are embodiment 1 respectively
TEM and SEM figure, (A2), (B2) be respectively embodiment 2 TEM and SEM figure, (A3), (B3) be respectively embodiment 3 TEM and
SEM figure；
Fig. 3 is hydridization colloidal particle prepared by the present invention to ultraviolet permeability figure；
Fig. 4 is degradation rate figure of the hydridization colloidal particle prepared by the present invention to rhodamine；
Fig. 5 is hydridization colloidal particle prepared by the present invention to DPPH radicals scavenging rate diagram；
Fig. 6 is emulsifying effectiveness figure of the hydridization colloidal particle prepared by the present invention to different cosmetic oils.
Specific embodiment
The light degradation rate test of rhodamine B:
Specific experiment operating method: rhodamine B is added to ZnO, QAC/L-Cys/ZnO-5, QAC/L-Cys/ZnO-7.5
And in QAC/L-Cys/ZnO-10 colloidal particle solution, makes its concentration to 0.1mg/mL, difference is irradiated to it with ultraviolet lamp
Time takes sample liquids 10mL, is centrifugated at 10000r/min, measures absorbance A of the supernatant liquor at 554nm, really
Determine the concentration of rhdamine B in solution, and calculates the degradation rate of rhodamine B by formula (1).
Degradation rate (%)=[(A0-A)/A0] × 100% (1)
In formula: A0, A be respectively rhodamine B solution before and after light processing absorbance.
Free radical (DPPH, OH, O2) elimination efficiency figure test:
The measurement of DPPH clearance rate: 1,1- diphenyl -2- trinitrophenyl-hydrazine (DPPH) is a kind of artificial synthesized with single electron
Free radical centered on nitrogen, what it can be highly stable is present in alcoholic solution and presents purple, has strong absorb at 517nm
Peak.When DPPH and antioxidant exist simultaneously, DPPH can absorb the electronics or hydrogen atom of an antioxidant institute band,
It matches to form a more stable leuco-compounds with the lone pair electrons of oneself institute's band, the number of free radical can be become by color
Change the photometer that can accurately and quickly be split to detect.DPPH clearance rate is because of its advantage such as convenient, fast, stable, extensively
Evaluation for antioxidant Scavenging ability.
Referring to the method for Zhou Hong, sample solution 0.5mL is taken, is separately added into 8 × 10-5mol L-1DPPH dehydrated alcohol it is molten
Liquid 2.5mL is uniformly mixed, and 45min is reacted in shading at room temperature, is centrifuged 10min under the conditions of 4000r/min, is measured and is inhaled at 517nm
Shading value, each sample survey is parallel three times, and DPPH clearance rate is calculated by formula 2.
In formula: A0Control group (0.5mL water+2.5mL DPPH solution) absorbance value；AiSample sets (0.5mL sample solution
+ 2.5mL DPPH solution) absorbance value；AjBlank group (0.5mL sample solution+2.5mL ethanol solution) absorbance value.
The measurement of OH clearance rate: hydroxyl radical free radical experiment is removed by removing Fe2+/H2O2OH in system is anti-oxidant to determine
Peptide removes hydroxyl radical free radical ability.It is slightly changed referring to the method for Wu Yue, sequentially adds 2mL 9mmol L-1FeSO4Solution,
2mL 9mmol L-1Salicylic acid-ethanol solution, 2mL anti-oxidation peptide solution is eventually adding 2mL in the test tube of 10mL
8.8mmol L-1H2O2Solution vibrates 1h in 37 DEG C of water-baths.It is compared simultaneously using deionized water as blank.At 536nm
The absorbance value of measurement solution, parallel 3 times.Hydroxyl radical free radical clearance rate is calculated with following formula 3:
In formula: AoFor the absorbance of blank control liquid；AsFor the absorbance that sample is added.
O2Clearance rate measurement: the experiment measures ultra-oxygen anion free radical clearance rate using pyrogallol method.Referring to Zhou Xu
Intelligent method is slightly changed, and 0.3mL sample solution is added in 10mL tool plug test tube and 5mL Tris-HCl (pH=8.2) is buffered
Solution, the water-bath 20min at 37 DEG C.0.3mL 7.5mmol L is added in tool plug test tube-1Pyrogallol solution, oscillation is equal
It is even, it is primary that its absorbance value is surveyed every 5s at 320nm rapidly, reacts 80s.It is plotted against time with absorbance, slope is sample
Product solution mouse thymus cells rate As.Sample is replaced with 0.3mL Tris-HCl buffer solution, measures neighbour according to the above method
Benzenetriol autoxidation rate Ao, in parallel three times.Ultra-oxygen anion free radical clearance rate is calculated by formula 4:
In formula: AoFor the absorbance of blank control liquid；AsFor the absorbance after sample is added.
The invention will be further described with reference to embodiments, but the present invention is not limited thereto.
Embodiment 1:
The preparation of nano zine oxide/n-trimethyl chitosan chloride hybrid nanomaterial: compound concentration is 3mg mL-10.5wt%
N-trimethyl chitosan chloride (QAC) aqueous solution 20mL, 3mg mL-1L-cysteine aqueous solution 20mL mixes the two in equal volume, then
Nanometer zinc oxide precursor is added, makes its concentration 2mg mL-1, stirring at room temperature for 24 hours is uniformly mixed it, finally with 0.5M's
It is 7 that NaOH, which adjusts pH value of solution, and colourless solution shows blue opalescence, as required nano zine oxide/n-trimethyl chitosan chloride hydridization
Nano particle (QAC/L-Cys/ZnO-2).
Embodiment 2:
The preparation of nano zine oxide/n-trimethyl chitosan chloride hybrid nanomaterial: compound concentration is 3mg mL-10.5wt%
QAC aqueous solution 20mL, 3mg mL-1The two is mixed in equal volume, adds nano zine oxide by L-cysteine aqueous solution 20mL
Presoma makes its concentration 4mg mL-1, stirring at room temperature for 24 hours is uniformly mixed it, finally adjusts pH value of solution with the NaOH of 0.5M
It is 7, colourless solution shows blue opalescence, as required nano zine oxide/n-trimethyl chitosan chloride hybrid nanomaterial (QAC/L-
Cys/ZnO-4)。
Embodiment 3:
The preparation of nano zine oxide/n-trimethyl chitosan chloride hybrid nanomaterial: compound concentration is 3mg mL-10.5wt%
QAC aqueous solution 20mL, 3mg mL-1The two is mixed in equal volume, adds nano zine oxide by L-cysteine aqueous solution 20mL
Presoma makes its concentration 6mg mL-1, stirring at room temperature for 24 hours is uniformly mixed it, finally adjusts pH value of solution with the NaOH of 0.5M
It is 7, colourless solution shows blue opalescence, as required nano zine oxide/n-trimethyl chitosan chloride hybrid nanomaterial (QAC/L-
Cys/ZnO-6)。
Comparative example 1:
Compound concentration is 1mg mL-1Chitosan aqueous solution 60mL, be added nano zine oxide 60mg, add 120mg friendship
Join agent sodium tripolyphosphate (TPP, QAC:ZnO:TPP=1:1:2), be ultrasonically treated 30min after magnetic agitation 15min, then by sample
It is centrifuged (4000rpm, 5 minutes), distillation water washing precipitating is twice to get CS zinc oxide；Before further test, by them
Directly it is resuspended in water.
Embodiment 4 is tested for the property above-mentioned gained hybrid nanomaterial:
The In situ ATR-FTIR of QAC, ZnO, L-cysteine and QAC/L-Cys/ZnO hydridization colloidal particle is tested:
Electrostatic interaction and L-cysteine and ZnO in QAC in protonated amino and hydroxyl and L-cysteine between anionic carboxyl it
Between complexing can induce form QAC/L-Cys/ZnO hydridization colloidal particle.Pure QAC, L-cysteine, ZnO and hybridized glue
The FTIR spectrogram of body particle illustrates to form hybrid in mixed process, as Fig. 1 it is infrared shown in, 1658cm in QAC spectrogram-1It is amide
I stretching vibration peak with carbonyl (C=O), and 1576cm-1It is amino N-H bending vibration in II band of amide and deacetylation unit
Combination.3182cm in L-cysteine spectrogram-1It is hydroxyl and-NH on carboxyl2Characteristic peak, 2537cm-1For the feature of-SH
Peak, the characteristic peak of the upper hydroxyl of ZnO are 3416cm-1.In QAC/ZnO spectrogram ,-SH characteristic peak disappears, it was demonstrated that sulfydryl and nano oxygen
Change zinc interaction, 3300cm-1Characteristic peak broadens and becomes strong, is the generation because of hydrogen bond, while 1037cm-1It is glucosides on QAC
The characteristic peak of key (C-O-C), it was demonstrated that successfully prepare QAC/L-Cys/ZnO hydridization colloidal particle.
Gained hybrid nanomaterial carries out properties of product, as shown in table 1:
1 hybrid nanomaterial properties of product of table
As shown in Table 1, nano particle diameter obtained by comparative example is 178nm, and embodiment 1,2,3 obtained hydridization colloid grains
The hybrid nanomaterial of son preparation is (Fig. 2) spherical in shape, and respectively in 100nm, 120nm, 150nm or so, granular size can subtract partial size
Small by 15.7%, preferable up to 43.8%, dispersion is more uniform；
From the figure 3, it may be seen that individually QAC and L-cysteine and the simple mixed solution of the two are in 230-420nm wave band
Transmitance be 80% or so, transmitance is higher, otherwise absorption of UV is lower, and the hybrid nanomaterial prepared penetrates
Rate significantly reduces, and increases with the increase of nano oxidized zinc concentration, and maximum transmission of the present invention in wave band can be down to
10%, illustrate that there are preferable UV absorbing properties；
Nano zine oxide is 95% (Fig. 4) to the degradation rate of rhodamine B after 5h, as shown in Table 1, by embodiment 1,2,3
The photocatalytic activity of obtained hydridization colloidal particle is substantially reduced, and only 1.5%, 3%, 4.6%, and the photocatalysis of comparative example 1
Activity is larger, is 12.7%, illustrates that nano zine oxide can effectively be shielded by coating nano zine oxide using n-trimethyl chitosan chloride
Photocatalytic activity, more-NH on n-trimethyl chitosan chloride2And the active Hydrogen Energy high-efficient cleaning on-OH removes free radical, thus significantly
Reduce its photocatalytic activity；
In addition, after 24h, the hydridization colloidal particle obtained by embodiment 1 is to DPPH, OH, O2The maximum of three kinds of free radicals
Clearance rate is respectively 81.3%, 46.8%, 60.2%；The hydridization colloidal particle obtained by embodiment 2 is to DPPH, OH, O2Three kinds
The maximal clearance of free radical is respectively 80.9%, 40.2%, 57.9%；The hydridization colloidal particle pair obtained by embodiment 3
DPPH,OH,O2The maximal clearance of three kinds of free radicals is respectively 78.1%, 36.9%, 52.6%；The nanometer that comparative example obtains
Grain is to DPPH, OH, O2The maximal clearance of three kinds of free radicals is respectively 79.7%, 26.0%, 37.3%, elimination efficiency all compared with
It is low, illustrate that hydridization colloidal particle of the present invention all has the function of preferable radicals scavenging, skin can be made from the damage of free radical；
It will be appreciated from fig. 6 that gained QAC/ZnO-6 hydridization colloidal particle can also stablize saualane, palm fibre in addition to it can stablize white oil
A variety of cosmetic oils such as the different monooctyl ester of palmitic acid acid, olive oil, wherein being that oil is mutually made with saualane, isobutyl palmitate, olive oil
Placement two months can be stablized by obtaining emulsion.Illustrate that the colloidal particle has certain universality, has in cosmetic field potential
Applying value.
Above-described embodiment is used to illustrate the present invention, rather than limits the invention, in spirit and right of the invention
It is required that protection scope in, to any modifications and changes for making of the present invention, fall within protection scope of the present invention.
Claims (10)
1. a kind of nano zine oxide/cationic polysaccharide hybrid nanomaterial preparation method, which is characterized in that the method packet
It includes:
(1) cationic polysaccharide solution and acid solution containing sulfhydryl amino are mixed, nanometer zinc oxide precursor is added, after being completely dissolved
Obtain cationic polysaccharide/containing mercaptoamino acid/nanometer zinc oxide precursor mixed solution；
(2) aqueous alkali is added to above-mentioned mixed solution to adjust, solution shows blue opalescence, obtains hybrid nanomaterial.
2. the method according to claim 1, wherein the cationic polysaccharide and the quality containing mercaptoamino acid are dense
Degree is than being (0.5~6): 1.
3. the method according to claim 1, wherein the nanometer zinc oxide precursor with containing mercaptoamino acid with
Mass concentration ratio be (0.1~6): 1.
4. the method according to claim 1, wherein the concentration of the cationic polysaccharide is 1~6mg/mL.
5. the method according to claim 1, wherein the concentration of the nanometer zinc oxide precursor be 0.5~
10mg/mL。
6. the method according to claim 1, wherein the concentration of aqueous solution containing mercaptoamino acid is 2~4mg/
mL。
7. the nano zine oxide that any the method for claim 1-6 is prepared/cationic polysaccharide hybrid nanomaterial.
8. a kind of cosmetic product, which is characterized in that received comprising nano zine oxide/cationic polysaccharide hydridization described in claim 7
Rice grain.
9. cosmetic product according to claim 8, which is characterized in that including cosmetics oil or lotion or cream.
10. nano zine oxide as claimed in claim 7/cationic polysaccharide hybrid nanomaterial is cosmetics are sun-proof or uvioresistant is inhaled
Receive the application in Material Field.
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