CN112206174A - Hydrogenated carbon nanotube gel, preparation method thereof and skin care product - Google Patents
Hydrogenated carbon nanotube gel, preparation method thereof and skin care product Download PDFInfo
- Publication number
- CN112206174A CN112206174A CN202011214670.5A CN202011214670A CN112206174A CN 112206174 A CN112206174 A CN 112206174A CN 202011214670 A CN202011214670 A CN 202011214670A CN 112206174 A CN112206174 A CN 112206174A
- Authority
- CN
- China
- Prior art keywords
- carbon nano
- nano tube
- hydrogenated
- carbon nanotube
- skin care
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 93
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 92
- -1 hydroxyl carbon nano tube Chemical compound 0.000 claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000839 emulsion Substances 0.000 claims abstract description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 5
- 238000001879 gelation Methods 0.000 claims abstract description 4
- 230000000640 hydroxylating effect Effects 0.000 claims abstract description 4
- 239000002048 multi walled nanotube Substances 0.000 claims description 39
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 239000000047 product Substances 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- 230000000694 effects Effects 0.000 claims description 16
- 239000012065 filter cake Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000003963 antioxidant agent Substances 0.000 claims description 7
- 230000003078 antioxidant effect Effects 0.000 claims description 7
- 239000002109 single walled nanotube Substances 0.000 claims description 7
- 230000003110 anti-inflammatory effect Effects 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000006210 lotion Substances 0.000 claims description 5
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 230000002087 whitening effect Effects 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000006071 cream Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 230000001815 facial effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 7
- 239000011148 porous material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 33
- 230000000052 comparative effect Effects 0.000 description 21
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 19
- 229910003472 fullerene Inorganic materials 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 239000012153 distilled water Substances 0.000 description 18
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 14
- 238000002835 absorbance Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 10
- 210000004027 cell Anatomy 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 8
- 150000003254 radicals Chemical class 0.000 description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 7
- 235000006708 antioxidants Nutrition 0.000 description 6
- 230000033444 hydroxylation Effects 0.000 description 6
- 238000005805 hydroxylation reaction Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 5
- 229930003268 Vitamin C Natural products 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 235000019154 vitamin C Nutrition 0.000 description 5
- 239000011718 vitamin C Substances 0.000 description 5
- 206010061218 Inflammation Diseases 0.000 description 4
- 230000002292 Radical scavenging effect Effects 0.000 description 4
- 239000012131 assay buffer Substances 0.000 description 4
- 238000012258 culturing Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 4
- 230000004054 inflammatory process Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 108010057466 NF-kappa B Proteins 0.000 description 3
- 102000003945 NF-kappa B Human genes 0.000 description 3
- 108700008625 Reporter Genes Proteins 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 102000040945 Transcription factor Human genes 0.000 description 3
- 108091023040 Transcription factor Proteins 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- WHNFPRLDDSXQCL-UAZQEYIDSA-N α-msh Chemical compound C([C@@H](C(=O)N[C@@H](CO)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CC=1NC=NC=1)C(=O)N[C@@H](CC=1C=CC=CC=1)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)NCC(=O)N[C@@H](CCCCN)C(=O)N1[C@@H](CCC1)C(=O)N[C@@H](C(C)C)C(N)=O)NC(=O)[C@H](CO)NC(C)=O)C1=CC=C(O)C=C1 WHNFPRLDDSXQCL-UAZQEYIDSA-N 0.000 description 3
- 239000005089 Luciferase Substances 0.000 description 2
- 102400000740 Melanocyte-stimulating hormone alpha Human genes 0.000 description 2
- 101710200814 Melanotropin alpha Proteins 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- UREBDLICKHMUKA-CXSFZGCWSA-N dexamethasone Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)CO)(O)[C@@]1(C)C[C@@H]2O UREBDLICKHMUKA-CXSFZGCWSA-N 0.000 description 2
- 229960003957 dexamethasone Drugs 0.000 description 2
- 239000002158 endotoxin Substances 0.000 description 2
- 230000002757 inflammatory effect Effects 0.000 description 2
- 229920006008 lipopolysaccharide Polymers 0.000 description 2
- 201000001441 melanoma Diseases 0.000 description 2
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000007845 reactive nitrogen species Substances 0.000 description 2
- 239000003642 reactive oxygen metabolite Substances 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- 230000019491 signal transduction Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- MZOFCQQQCNRIBI-VMXHOPILSA-N (3s)-4-[[(2s)-1-[[(2s)-1-[[(1s)-1-carboxy-2-hydroxyethyl]amino]-4-methyl-1-oxopentan-2-yl]amino]-5-(diaminomethylideneamino)-1-oxopentan-2-yl]amino]-3-[[2-[[(2s)-2,6-diaminohexanoyl]amino]acetyl]amino]-4-oxobutanoic acid Chemical compound OC[C@@H](C(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CCCN=C(N)N)NC(=O)[C@H](CC(O)=O)NC(=O)CNC(=O)[C@@H](N)CCCCN MZOFCQQQCNRIBI-VMXHOPILSA-N 0.000 description 1
- VNXWANZMRATDQM-UHFFFAOYSA-N 2-(2-phenylethyl)benzene-1,3-diol Chemical compound OC1=CC=CC(O)=C1CCC1=CC=CC=C1 VNXWANZMRATDQM-UHFFFAOYSA-N 0.000 description 1
- 102000003777 Interleukin-1 beta Human genes 0.000 description 1
- 108090000193 Interleukin-1 beta Proteins 0.000 description 1
- 102000004889 Interleukin-6 Human genes 0.000 description 1
- 108090001005 Interleukin-6 Proteins 0.000 description 1
- WTDRDQBEARUVNC-LURJTMIESA-N L-DOPA Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-LURJTMIESA-N 0.000 description 1
- WTDRDQBEARUVNC-UHFFFAOYSA-N L-Dopa Natural products OC(=O)C(N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-UHFFFAOYSA-N 0.000 description 1
- 108060001084 Luciferase Proteins 0.000 description 1
- 108060008682 Tumor Necrosis Factor Proteins 0.000 description 1
- 102000000852 Tumor Necrosis Factor-alpha Human genes 0.000 description 1
- 102000003425 Tyrosinase Human genes 0.000 description 1
- 108060008724 Tyrosinase Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000021164 cell adhesion Effects 0.000 description 1
- 230000032677 cell aging Effects 0.000 description 1
- 239000013592 cell lysate Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940044683 chemotherapy drug Drugs 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 210000001985 kidney epithelial cell Anatomy 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004768 lowest unoccupied molecular orbital Methods 0.000 description 1
- 238000003670 luciferase enzyme activity assay Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008099 melanin synthesis Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000013612 plasmid Substances 0.000 description 1
- 238000012802 pre-warming Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000011506 response to oxidative stress Effects 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 230000002103 transcriptional effect Effects 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
-
- 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
- A61K8/04—Dispersions; Emulsions
- A61K8/042—Gels
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Dermatology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- Nanotechnology (AREA)
- Birds (AREA)
- Dispersion Chemistry (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Pain & Pain Management (AREA)
- Rheumatology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Pharmacology & Pharmacy (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a hydrogenated carbon nanotube gel, a preparation method thereof and a skin care product, and belongs to the technical field of skin care products. The preparation method comprises the following steps: a) hydroxylating the carbon nano tube to obtain a hydroxyl carbon nano tube; b) and (3) carrying out hydrogenation gelation on the hydroxyl carbon nano tube to obtain hydrogenated carbon nano tube gel. The hydrogenated carbon nanotube gel provided by the invention is mainly used for preparing skin care products, can obviously improve the dispersibility of the carbon nanotubes in media such as emulsion and the like, and can also greatly improve the reducibility of the carbon nanotubes because a large amount of hydrogen can be stored in the pore walls of the carbon nanotubes.
Description
Technical Field
The invention belongs to the technical field of skin care products, and particularly relates to a hydrogenated carbon nanotube gel, a preparation method thereof and a skin care product.
Background
When the oxidation and antioxidation effects in the human body are unbalanced, a large amount of oxidation products, such as Reactive Oxygen Species (ROS) and Reactive Nitrogen Species (RNS), are generated. The oxidative stress reaction caused by chemotherapeutic drugs, external radiation and the physiological metabolism in the body promotes the generation of oxidation products in the body and damages cells of the human body, which is one of the important factors causing diseases and aging. Studies have shown that as free radicals decrease in vivo, the rate of cellular aging slows, skin elasticity increases, and human aging is delayed.
Carbon nanotubes were discovered in 1985, and have a large number of carbon-carbon double bonds and LUMO orbitals, which can absorb electrons and react with free radicals, but the reducibility is far from meeting the requirement, and the dispersibility is poor, so that the carbon nanotubes are difficult to be directly used as antioxidant products.
Disclosure of Invention
The invention provides a hydrogenated carbon nanotube gel, a preparation method thereof and a skin care product, and aims to solve the problems that the reducibility of a carbon nanotube cannot meet the requirement, the dispersibility is poor and the like.
The invention provides a preparation method of hydrogenated carbon nanotube gel, which comprises the following steps:
a) hydroxylating the carbon nano tube to obtain a hydroxyl carbon nano tube;
b) and (3) carrying out hydrogenation gelation on the hydroxyl carbon nano tube to obtain hydrogenated carbon nano tube gel.
Further, the carbon nanotubes comprise single-walled carbon nanotubes or multi-walled carbon nanotubes;
preferably, the carbon nanotubes are multi-walled carbon nanotubes.
Further, the step a) includes:
a1) dissolving carbon nano tubes in a hydrochloric acid solution, performing ultrasonic treatment, reacting, cooling to room temperature, filtering reaction liquid, washing a filter cake, and drying to obtain pretreated carbon nano tubes;
a2) under the condition of no oxygen, the pretreated carbon nano tube and NaAlO are mixed2Adding the mixture into a solvent, filtering reaction liquid after reaction, washing a filter cake, and drying to obtain the hydroxyl carbon nanotube.
Further, the step b) comprises:
and (3) placing the hydroxyl carbon nano tube into a high-pressure reaction kettle, respectively replacing with nitrogen and hydrogen, and pressurizing with hydrogen to obtain the hydrogenated hydroxyl carbon nano tube.
Further, in step a1),
the addition amount of the carbon nano tube and the hydrochloric acid solution is (0.5-1.5) g: (100-300) mL; wherein the concentration of the hydrochloric acid solution is 6 mol/L;
the ultrasonic time is 0.5-2 h;
the reaction temperature is 90-95 ℃, and the reaction time is 15-30 h;
the drying temperature is 70-90 ℃, and the drying time is 18-30 h.
Further, in step a2),
the pre-treated carbon nano tube and NaAlO2The mass ratio of (0.1-0.3) to (0.3-0.9);
the reaction time is 10-15 hours, and the reaction temperature is 20-30 ℃;
the drying temperature is 70-90 ℃, and the drying time is 18-30 h.
Further, in the step b),
the pressure of hydrogen pressurization is 0.1 Mpa;
the time for pressurizing the hydrogen is 0.5-2 h.
The invention also provides the hydrogenated carbon nanotube gel prepared by any one of the preparation methods.
The invention also provides a skin care product which comprises any one of the hydrogenated carbon nanotube gel.
Further, the skin care product has at least one of antioxidant, whitening, anti-inflammatory and repairing effects;
preferably, the skin care product comprises essence, skin lotion, emulsion, cream and facial mask.
The invention has the following advantages:
the preparation method of the hydrogenated carbon nanotube gel provided by the invention is characterized in that the carbon nanotube is hydroxylated and then hydrogenated to form the hydrogenated carbon nanotube gel. The gel can obviously improve the dispersibility of the carbon nano tube in media such as emulsion and the like, and meanwhile, the hydrogen can be stored in the pore wall of the carbon nano tube in a large amount, so that the reducibility of the carbon nano tube can be greatly improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a comparison of the upper liquid volumes obtained by evaluating the aqueous solution of hydrogenated multi-walled carbon nanotubes of example 1 of the present invention and the aqueous solution of ordinary multi-walled carbon nanotubes of comparative example 1 by the gravity sedimentation method.
FIG. 2 shows the absorbance values of the supernates of the hydrogenated multi-walled carbon nanotube aqueous solution of example 1 and the conventional multi-walled carbon nanotube aqueous solution of comparative example 1 measured by spectrophotometry.
Fig. 3 shows the results of measuring the scavenging ability (. about.p <0.01) of the free radicals of the products to be measured in examples 1 to 2 and comparative examples 1 to 3 of the present invention.
FIG. 4 shows the results of measuring the ability of the hydrogenated carbon nanotubes obtained in example 1 of the present invention to scavenge hydroxyl radicals of fullerene in comparative example 3.
Figure 5 shows the effect of the product of example 1 of the invention and comparative examples 1, 3 on the inflammatory signaling pathway (. about.p < 0.01).
FIG. 6 shows the effect of the products of example 1 and comparative examples 1 and 3 according to the invention on tyrosinase activity (. about.P <0.01)
Figure 7 shows the effect of the products of example 1 of the invention and comparative examples 1, 3, 4 on melanin production (. about.p < 0.01).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
In the prior art, hydrogen has reducibility, can neutralize oxygen free radicals, especially hydroxyl free radicals which have great threat to human bodies, and can inhibit the expression of IL-6, IL-1 beta and TNF-alpha in extracorporeal circulation and relieve inflammatory reaction. However, the use of hydrogen alone tends to be too effective and unstable.
The invention skillfully combines the carbon nano tube and the hydrogen with reducibility, not only can solve the problem of poor reducibility of the carbon nano tube when the carbon nano tube is used alone, but also can ensure that the carbon nano tube exists in a medium uniformly and stably.
An embodiment of the present invention provides a method for preparing a hydrogenated carbon nanotube gel, including the following steps:
a) hydroxylating the carbon nano tube to obtain a hydroxyl carbon nano tube;
b) and (3) carrying out hydrogenation gelation on the hydroxyl carbon nano tube to obtain hydrogenated carbon nano tube gel.
In the preparation method of the hydrogenated carbon nanotube gel provided by the embodiment of the invention, the carbon nanotube is hydroxylated and then hydrogenated to form the hydrogenated carbon nanotube gel. The gel can obviously improve the dispersibility of the carbon nano tube in media such as emulsion and the like, and meanwhile, the hydrogen can be stored in the pore wall of the carbon nano tube in a large amount, so that the reducibility of the carbon nano tube can be greatly improved.
In an embodiment of the present invention, the carbon nanotube includes a single-walled carbon nanotube or a multi-walled carbon nanotube. Preferably, the carbon nanotubes are multi-walled carbon nanotubes. The multi-walled carbon nanotube of the embodiment of the invention is a carbon nanotube with two layers of walls and more than two layers of walls. The multi-walled carbon nanotube has a plurality of walls, so that hydrogen is stored more and the reducibility of hydrogen can be exerted more.
In an embodiment of the present invention, the step a) includes:
a1) dissolving carbon nano tubes in a hydrochloric acid solution, performing ultrasonic treatment, reacting, cooling to room temperature, filtering reaction liquid, washing a filter cake, and drying to obtain pretreated carbon nano tubes;
a2) under the oxygen-free condition, the pre-treated carbon nano tube obtained in the step a1) and NaAlO2Adding the mixture into a solvent, filtering reaction liquid after reaction, washing a filter cake, and drying to obtain the hydroxyl carbon nanotube.
In an embodiment of the present invention, in step a1), the addition amount of the carbon nanotubes and the hydrochloric acid solution is (0.5-1.5) g: (100-300) mL; wherein the concentration of the hydrochloric acid solution is 6 mol/L. The hydrochloric acid solution is an aqueous solution of hydrochloric acid.
In an embodiment of the invention, in the step a1), the ultrasonic time is 0.5-2 hours.
In an embodiment of the invention, in the step a1), the reaction temperature is 90-95 ℃, and the reaction time is 15-30 hours.
In an embodiment of the invention, in the step a1), the drying temperature is 70-90 ℃, and the drying time is 18-30 hours.
In the embodiment of the invention, in the step a1), the filter cake is washed by distilled water for multiple times until the filtrate is neutral. In the step a1), the reaction solution is filtered mainly to filter the filtrate and remove iron ions and excessive hydrochloric acid in the carbon nanotubes.
In one embodiment of the present invention, in the step a2), the carbon nanotubes and the NaAlO are pretreated2The mass ratio of (0.1-0.3) to (0.3-0.9).
In an embodiment of the present invention, in the step a2), the addition amount of the solvent is: the solvent is (0.1-0.3) g: (20-60) ml. Wherein the solvent is tetrahydrofuran.
In an embodiment of the invention, in the step a2), the reaction time is 10-15 hours; the reaction temperature is 20-30 ℃.
In an embodiment of the invention, in the step a2), the drying temperature is 70-90 ℃, and the drying time is 18-30 hours.
In an embodiment of the invention, in the step a2), the washing is performed 1-5 times by using ethanol and distilled water respectively. In the step a2), the reaction solution obtained by the reaction can be diluted by 20-30 times with distilled water.
In an embodiment of the present invention, the step b) includes:
and (3) placing the hydroxyl carbon nano tube into a stainless steel high-pressure reaction kettle, respectively replacing with nitrogen and hydrogen, and pressurizing with hydrogen to obtain the hydrogenated hydroxyl carbon nano tube.
In one embodiment of the present invention, in step b), the pressure of hydrogen pressurization is 0.1 Mpa; the time for pressurizing the hydrogen is 0.5-2 h.
In one embodiment of the present invention, when nitrogen and hydrogen are used for replacement, nitrogen may be used for replacement for 1 to 4 times, and hydrogen may be used for replacement for 1 to 4 times. High-purity nitrogen and high-purity (99.999%) hydrogen are respectively adopted for replacement so as to remove air in the reaction kettle.
An embodiment of the invention also provides the hydrogenated carbon nanotube gel prepared by any one of the preparation methods.
An embodiment of the present invention further provides a skin care product, including the hydrogenated carbon nanotube gel.
Specifically, the skin care product has at least one of antioxidant, whitening, anti-inflammatory and repairing effects.
Preferably, the skin care product may include essence, skin lotion, cream, mask, etc. Other external preparations having skin care effects are also suitable.
Furthermore, the existence form of the hydrogenated carbon nanotube gel in the skin care product is not limited. For example, in the form of an aqueous lotion, a water-in-oil or oil-in-water emulsion, an oil or oleyl lotion, a vesicular dispersion of an anionic or nonionic amphiphilic lipid, an aqueous gel, a hydroalcoholic gel, an alcoholic or oleyl gel, a solid stick or an aerosol, and the like.
Specifically, the skin care product has at least one of antioxidant, anti-inflammatory, repairing and whitening functions.
The hydrogenated carbon nanotube gel obtained in the embodiment of the invention has obviously higher free radical removal capacity and melanin removal capacity than fullerene, and has antioxidant and whitening functions. Because of stable combination with hydrogen, the anti-inflammatory and repairing effects of the nano-carbon tube are obviously superior to those of the common carbon nano-tube.
The present invention will be described in detail with reference to examples.
Example 1A preparation method of hydrogenated carbon nanotube gel (HS-MWCNT) comprises the following steps:
respectively carrying out hydroxylation and hydrogelation treatment on the carbon nano tube in sequence;
the carbon nano-tube is a multi-wall carbon nano-tube.
The hydroxylation treatment of the carbon nano tube comprises the following steps:
0.5 g of multi-walled carbon nanotubes are dissolved in 200ml of 6mol/L hydrochloric acid aqueous solution and subjected to ultrasonic treatment for 1 hour. Then reacted at 95 ℃ for 20 hours and then cooled to room temperature. Filtering the reaction solution, filtering the filtrate, and removing iron ions and redundant hydrochloric acid in the carbon nano tube. The filter cake was washed several times with distilled water until the filtrate was neutral. The filter cake was then dried in an oven at 80 ℃ for 24 hours.
Subsequently, 20ml of freshly distilled tetrahydrofuran were deoxygenated with nitrogen for 60 minutes, 0.15 g of the previously treated carbon nanotubes and 0.4 g of NaAlO2The resulting mixture was poured into treated tetrahydrofuran, and stirred at room temperature for 10 hours. After completion of the reaction, the reaction mixture was poured into 500ml of distilled water and stirred for 1 hour. Then filtered and washed three times with ethanol and distilled water, respectively. And drying the filter cake in an oven at 80 ℃ for 24 hours to obtain the hydroxyl carbon nanotube.
The method for carrying out hydrogelation on the pretreated carbon nanotube comprises the following steps:
1 g of hydroxyl carbon nano tube is placed in a stainless steel high-pressure reaction kettle, high-purity nitrogen is used for replacing for 3 times to remove air in the reaction kettle, and high-purity (99.999%) hydrogen is used for replacing for 3 times. And after the replacement is completed, keeping the hydrogen pressure at 0.1MPa, and pressurizing for 1 hour to obtain the hydrogenated hydroxyl carbon nano tube.
Example 2Preparation method of hydrogenated carbon nanotube gel (HS-SWCNT)
Also, example 1 is different in that single-walled carbon nanotubes are used instead of multi-walled carbon nanotubes.
Example 3A preparation method of hydrogenated carbon nanotube gel comprises the following steps:
respectively carrying out hydroxylation and hydrogelation treatment on the carbon nano tube in sequence;
the carbon nano-tube is a multi-wall carbon nano-tube.
The hydroxylation treatment of the carbon nano tube comprises the following steps:
1 g of multi-walled carbon nano-tube is dissolved in 250ml of 6mol/L hydrochloric acid aqueous solution and is subjected to ultrasonic treatment for 1 hour. Then reacted at 95 ℃ for 22 hours, and then cooled to room temperature. Filtering the reaction solution, filtering the filtrate, and removing iron ions and redundant hydrochloric acid in the carbon nano tube. The filter cake was washed several times with distilled water until the filtrate was neutral. The filter cake was then dried in an oven at 80 ℃ for 24 hours.
Subsequently, 20ml of freshly distilled tetrahydrofuran were deoxygenated with nitrogen for 60 minutes, 0.2 g of the previously treated carbon nanotubes and 0.5 g of NaAlO2The resulting mixture was poured into treated tetrahydrofuran, and stirred at room temperature for 10 hours. After completion of the reaction, the reaction mixture was poured into 500ml of distilled water and stirred for 1 hour. Then filtered and washed three times with ethanol and distilled water, respectively. And drying the filter cake in an oven at 80 ℃ for 24 hours to obtain the hydroxyl carbon nanotube.
The method for carrying out hydrogelation on the pretreated carbon nanotube comprises the following steps:
1 g of hydroxyl carbon nano tube is placed in a stainless steel high-pressure reaction kettle, high-purity nitrogen is used for replacing for 3 times to remove air in the reaction kettle, and high-purity (99.999%) hydrogen is used for replacing for 3 times. And after the replacement is completed, keeping the hydrogen pressure at 0.1MPa, and pressurizing for 1 hour to obtain the hydrogenated hydroxyl carbon nano tube.
Example 4
A preparation method of hydrogenated carbon nanotube gel (HS-MWCNT) comprises the following steps:
respectively carrying out hydroxylation and hydrogelation treatment on the carbon nano tube in sequence;
the carbon nanotube is a double-walled carbon nanotube.
The hydroxylation treatment of the carbon nano tube comprises the following steps:
0.8 g of multi-walled carbon nanotubes was dissolved in 230ml of 6mol/L aqueous hydrochloric acid and sonicated for 1 hour. Then reacted at 95 ℃ for 20 hours and then cooled to room temperature. Filtering the reaction solution, filtering the filtrate, and removing iron ions and redundant hydrochloric acid in the carbon nano tube. The filter cake was washed several times with distilled water until the filtrate was neutral. The filter cake was then dried in an oven at 80 ℃ for 24 hours.
Subsequently, 20ml of freshly distilled tetrahydrofuran were deoxygenated with nitrogen for 60 minutes, and 0.18 g of the previously treated carbon nanotubes and 0.6 g of NaAlO were taken2The resulting mixture was poured into treated tetrahydrofuran, and stirred at room temperature for 10 hours. After completion of the reaction, the reaction mixture was poured into 500ml of distilled water and stirred for 1 hour. Then filtered and washed three times with ethanol and distilled water, respectively. And drying the filter cake in a drying oven at 90 ℃ for 20 hours to obtain the hydroxyl carbon nanotube.
The method for carrying out hydrogelation on the pretreated carbon nanotube comprises the following steps:
1 g of hydroxyl carbon nano tube is placed in a stainless steel high-pressure reaction kettle, high-purity nitrogen is used for replacing for 3 times to remove air in the reaction kettle, and high-purity (99.999%) hydrogen is used for replacing for 3 times. And after the replacement is completed, keeping the hydrogen pressure at 0.1MPa, and pressurizing for 1 hour to obtain the hydrogenated hydroxyl carbon nano tube.
Comparative example 1
The same general multiwall carbon nanotube stock (MWCNT) as in example 1 was used directly without any treatment.
Comparative example 2
The same general single-walled carbon nanotube material (SWCNT) as in example 2 was used directly without any treatment.
Comparative example 3
Fullerene (fullerene) is a common active ingredient in skin care products used in the prior art. The fullerene is commercially available.
Comparative example 4
The active component Vitamin C (VC) of the skin care product is commonly used in the prior art. The vitamin C is commercially available.
Test example 1Evaluation of Dispersion stability
First, 100mL of 1mg/mL or 2mg/mL aqueous solution of the ordinary multi-walled carbon nanotube obtained in comparative example 1 and 1mg/mL or 2mg/mL aqueous solution of the hydrogenated multi-walled carbon nanotube obtained in example 1 were prepared, dispersed at room temperature by ultrasonic wave for 30min, and then evaluated by a gravity sedimentation method and a spectrophotometric method, respectively.
Evaluation by a gravity sedimentation method: after 3 times of 25mL of each sample were poured into a stoppered tube and allowed to stand for 8 hours, the supernatant was carefully poured out into a graduated cylinder and the volume V1 was read, the larger the value of V1, the more stable the dispersion was, and the average of the results obtained in 3 times was taken, and the results are shown in FIG. 1.
As can be seen from FIG. 1, the dispersion effect of HS-MWCNT is better and the volume of upper layer liquid is larger under the same mass concentration.
Evaluation by spectrophotometry: taking 1mL of the rest 25mL of supernatant in the gravity settling test, diluting the supernatant with deionized water properly, fixing the volume to a uniform volume, placing the supernatant in a cuvette, and detecting the light absorption value by using an ultraviolet spectrophotometer, wherein the result is shown in figure 2.
The absorbance of the supernatant of the suspension is in direct proportion to the dispersion and suspension stability of the sample, so that the change of the absorbance can directly reflect the dispersion effect of the sample. As can be taken from fig. 2, the instability of the conventional nanotube dispersion is very significant over time; although the absorbance value of the hydrogenated carbon nanotube dispersion system is slightly reduced, the overall stability of the hydrogenated carbon nanotube dispersion system is still obviously superior to that of the common carbon nanotube.
Test example 2Detection of antioxidant capacity
A DPPH (1, 1-diphenyl-2-trinitrophenylhydrazine) detection method is adopted, and specifically comprises the following steps:
firstly, preparing solutions to be detected with different concentrations, namely aqueous solutions of products to be detected in examples 1-2 and comparative examples 1-3 with different concentrations.
Secondly, accurately weighing 25mg of DPPH standard, dissolving with methanol and fixing the volume to 500mL, wherein the concentration of the solution is 0.05 mg/mL.
Then, the samples were added to the test tube with a stopper in the amount shown in Table 1, and after shaking up and reacting for 30 minutes, the absorbance values were measured at 517nm with reference to a mixture of 2.5mL of methanol and 0.5mL of distilled water.
Finally, the scavenging capacity of the solution to be tested for free radicals is calculated according to the formula S ═ 1- (Ai-Aj)/Ao, and the result is shown in FIG. 3.
TABLE 1
| Absorbance A | Configuration method and sample adding amount |
| A0 | 2.5mL of a 0.05mg/mL solution of DPPH in methanol +0.5mL of distilled water |
| Ai | 2.5mL of 0.05mg/mL DPPH methanol solution +0.5mL of solutions to be tested with different concentrations |
| Aj | 2.5mL of methanol solution +0.5mL of solutions to be tested with different concentrations |
| Blank space | 2.5mL of methanol solution +0.5mL of distilled water |
As can be seen from fig. 3, the DPPH test results show that the hydrogenated carbon nanotubes (HS-CNTs) have approximately at least 78% higher radical scavenging ability than fullerenes at the same mass concentration, and are also significantly higher than VC. Also, hydrogenated multi-walled carbon nanotubes are at least 50% higher than normal multi-walled carbon nanotubes. Therefore, the hydrogenated multi-walled carbon nanotube provided by the application has better oxidation resistance.
Test example 3Measurement of hydroxyl radical scavenging ability
The detection method specifically comprises the following steps:
preparing OH Assay buffer working solution: taking a proper amount of OH Assay buffer and H2O2Base solution, according to OH Assay buffer: h2O2The base liquid is 10 ml: mixing at a ratio of 15 μ L to obtain OH Assay buffer working solution, and storing at 4 deg.C in dark for 1 week.
Preparing OH extraction washing liquid: taking a proper amount of distilled water and OH extract liquor, and mixing the distilled water: OH extract 23: 1 to obtain the OH extraction washing liquid.
OH loading: a control tube, a measuring tube (the sample to be measured was the hydrogenated carbon nanotube obtained in example 1 and the fullerene in comparative example 3), and a pure sample tube were set in accordance with Table 2, and the solutions were sequentially added.
TABLE 2
OH determination method: adding 1.6ml of OH extraction cleaning solution into a control tube and a measuring tube, slightly and uniformly mixing, standing and layering, discarding the lower aqueous phase, adding newly prepared 2.4ml of OH extraction cleaning solution into the upper organic phase, standing and layering to obtain the upper liquid, namely the hydroxyl radical solution to be measured.
Taking a 96-well plate, adding the solutions of a control tube, a measuring tube and a pure sample tube into the 96-well plate, adjusting the solution to zero by using distilled water, measuring the absorbance at 420nm of the control hole and the measuring hole by using an enzyme-labeling instrument, and respectively recording the absorbance of the control tube, the absorbance of the sample and the absorbance of the measuring tube as AControl、A0、AMeasurement of。
OH clearance (%) by formula ((a)Measurement of-A0)-AControl)/AControlX 100 OH clearance of tissue samples was calculated and the results are shown in FIG. 4.
As shown in fig. 4, the hydroxyl radical scavenging ability of the hydrogenated carbon tube is about 1.4 times that of fullerene as proved by the test result of hydroxyl radical scavenging ability.
Test example 4Effect test of inflammatory factor Signal pathway
The method for detecting the dual-luciferase reporter gene comprises the following steps:
human kidney epithelial cell 293T was inoculated in 96-well plates at 37 ℃ with 5% CO2Culturing in an incubator until cells adhere to the wall, transfecting NF-kB reporter gene plasmids, continuously culturing for 24h, adding Dexamethasone (DXMS) with proper concentration, hydrogenated multi-wall carbon nanotubes (HS-MWCNT) obtained in example 1, common multi-wall carbon nanotubes (MWCNT) in comparative example 1, and fullerene (fullerene) in comparative example 3, and respectively incubating for 2 h. Then Lipopolysaccharide (LPS) is added to induce inflammatory reaction,after 4h of action, the cells were digested and the transcriptional activity of the NF- κ B transcription factor was determined according to the luciferase assay kit instructions. The results are shown in FIG. 5.
From FIG. 5, it is proved that fullerene, multi-walled carbon nanotube and hydrogenated carbon nanotube all have certain inhibition effect on NF-kB pathway of inflammation-related transcription factor by dual luciferase reporter gene.
Moreover, the effect of inhibiting the NF-kB channel of the transcription factor related to inflammation by the hydrogenated carbon nano tube under the same concentration is at least about 66 percent higher than that of the fullerene; after hydrogenation, the anti-inflammatory capability of the carbon nano tube is improved by at least 55 percent.
Test example 5Tyrosinase activity effect assay
The detection method specifically comprises the following steps:
mouse melanoma cells B16F10 were inoculated in a 96-well plate, cultured overnight in a 5% CO2 incubator at 37 ℃ and, after cell adhesion, replaced with fresh culture solutions of hydrogenated multi-walled carbon nanotubes (HS-MWCNTs) obtained in example 1, ordinary multi-walled carbon nanotubes (MWCNTs) obtained in comparative example 1, fullerenes (fullerenes) obtained in comparative example 3 and a positive drug 377 (phenethylresorcinol), respectively, and after further culturing for 48 hours, the culture solutions were discarded and washed 2 times with PBS (pH 7.4). 50 μ l of 1% TritonX-100 solution was added to each well, and the mixture was rapidly frozen at-80 ℃ for 30min, followed by thawing at room temperature to completely lyse the cells. After pre-warming at 37 ℃, 10 mu L of 1 percent L-DOPA solution is added for reaction for 2h at 37 ℃. The absorbance value at 490nm was measured in 4 replicate wells per concentration and averaged. The results are shown in FIG. 6.
As can be seen from fig. 6, by comparing the levels of melanin in the microenvironment of the cells treated with fullerene and hydrogenated carbon nanotubes, the ability of the hydrogenated carbon nanotubes to remove or inhibit melanin is about 45% higher than that of fullerene, and the ability of the hydrogenated carbon nanotubes at 4mg/mL to remove melanin is significantly better than that of 377 at 50 μ M.
Test example 6Determination of the ability to clear melanin
The detection method specifically comprises the following steps:
mouse melanoma cells B16F10 were seeded in 6-well plates at 37 ℃ with 5% CO2Culturing in an incubator overnight, and leaving the blank group untreated after the cells adhere to the wall; control groupAdding alpha-MSH; the positive medicines are divided into two groups, and alpha-MSH is added into the two groups, and Vc in a comparative example 4 and fullerene in a comparative example 3 are added into the two groups respectively; the experimental group was added with α -MSH and various concentrations of the common multi-walled carbon nanotubes of comparative example 1 and the hydrogenated multi-walled carbon nanotubes obtained in example 1. After adding the drug for 40-48h, collecting cells by trypsinization, and adding 60 mu L NaOH (2 mol/L). After lysis at 80 ℃ for 1h, the cell lysate was added to a 96-well plate and absorbance was measured at 490 nm. The results are shown in FIG. 7.
From fig. 7, it can be seen that, by comparing the levels of melanin in the microenvironment of the cells treated with fullerene and hydrogenated carbon nanotubes, the ability of the hydrogenated carbon nanotubes to remove or inhibit melanin is about 45% higher than that of fullerene, and the ability of the hydrogenated carbon nanotubes at 4mg/mL to remove melanin is significantly better than that of 50 μ M VC.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of hydrogenated carbon nanotube gel is characterized by comprising the following steps:
a) hydroxylating the carbon nano tube to obtain a hydroxyl carbon nano tube;
b) and (3) carrying out hydrogenation gelation on the hydroxyl carbon nano tube to obtain hydrogenated carbon nano tube gel.
2. The production method according to claim 1,
the carbon nanotubes comprise single-walled carbon nanotubes or multi-walled carbon nanotubes;
preferably, the carbon nanotubes are multi-walled carbon nanotubes.
3. The production method according to claim 1 or 2,
the step a) comprises the following steps:
a1) dissolving carbon nano tubes in a hydrochloric acid solution, performing ultrasonic treatment, reacting, cooling to room temperature, filtering reaction liquid, washing a filter cake, and drying to obtain pretreated carbon nano tubes;
a2) under the condition of no oxygen, the pretreated carbon nano tube and NaAlO are mixed2Adding the mixture into a solvent, filtering reaction liquid after reaction, washing a filter cake, and drying to obtain the hydroxyl carbon nanotube.
4. The production method according to claim 1,
the step b) comprises the following steps:
and (3) placing the hydroxyl carbon nano tube into a high-pressure reaction kettle, respectively replacing with nitrogen and hydrogen, and pressurizing with hydrogen to obtain the hydrogenated hydroxyl carbon nano tube.
5. The production method according to claim 3,
in the step a1), the step b,
the addition amount of the carbon nano tube and the hydrochloric acid solution is (0.5-1.5) g: (100-300) mL; wherein the concentration of the hydrochloric acid solution is 6 mol/L;
the ultrasonic time is 0.5-2 h;
the reaction temperature is 90-95 ℃, and the reaction time is 15-30 h;
the drying temperature is 70-90 ℃, and the drying time is 18-30 h.
6. The production method according to claim 3,
in the step a2), the step b,
the pre-treated carbon nano tube and NaAlO2The mass ratio of (0.1-0.3) to (0.3-0.9);
the reaction time is 10-15 h, and the reaction temperature is 20-30 ℃;
the drying temperature is 70-90 ℃, and the drying time is 18-30 h.
7. The production method according to any one of claims 1 to 3,
in the step b), the step (c),
the pressure of hydrogen pressurization is 0.1 Mpa;
the time for pressurizing the hydrogen is 0.5-2 h.
8. The hydrogenated carbon nanotube gel produced by the production method according to any one of claims 1 to 7.
9. A skin care product comprising the hydrogenated carbon nanotube gel of claim 8.
10. A skin care product according to claim 9,
the skin care product has at least one of antioxidant, whitening, anti-inflammatory and repairing effects;
preferably, the skin care product comprises essence, skin lotion, emulsion, cream and facial mask.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011214670.5A CN112206174A (en) | 2020-11-04 | 2020-11-04 | Hydrogenated carbon nanotube gel, preparation method thereof and skin care product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011214670.5A CN112206174A (en) | 2020-11-04 | 2020-11-04 | Hydrogenated carbon nanotube gel, preparation method thereof and skin care product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112206174A true CN112206174A (en) | 2021-01-12 |
Family
ID=74058172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011214670.5A Pending CN112206174A (en) | 2020-11-04 | 2020-11-04 | Hydrogenated carbon nanotube gel, preparation method thereof and skin care product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112206174A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113593A (en) * | 2013-02-26 | 2013-05-22 | 哈尔滨理工大学 | Preparation method of hydroxylated multi-wall carbon nanotube-polysilane composite material |
-
2020
- 2020-11-04 CN CN202011214670.5A patent/CN112206174A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113593A (en) * | 2013-02-26 | 2013-05-22 | 哈尔滨理工大学 | Preparation method of hydroxylated multi-wall carbon nanotube-polysilane composite material |
Non-Patent Citations (1)
| Title |
|---|
| 至本: "《至本美肌课堂微信公众号》", 15 May 2020 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tosun et al. | A composite SWNT–collagen matrix: characterization and preliminary assessment as a conductive peripheral nerve regeneration matrix | |
| Bo et al. | In vitro evaluation of cytotoxicity and oxidative stress induced by multiwalled carbon nanotubes in murine RAW 264.7 macrophages and human A549 lung cells | |
| CN112437752B (en) | Graphene products and cosmetic applications thereof | |
| Tonglairoum et al. | Fast-acting clotrimazole composited PVP/HPβCD nanofibers for oral candidiasis application | |
| Mianehrow et al. | Introducing a highly dispersed reduced graphene oxide nano-biohybrid employing chitosan/hydroxyethyl cellulose for controlled drug delivery | |
| CN111504956B (en) | Preparation of carbon quantum dot fluorescent probe and application of carbon quantum dot fluorescent probe in selective detection of active oxygen | |
| Nehru et al. | Electrochemical determination of caffeic acid in antioxidant beverages samples via a facile synthesis of carbon/iron-based active electrocatalyst | |
| CN104248992A (en) | Spherical diatomite mesoporous composite and supported catalyst, preparation method thereof and application thereof, and ethyl acetate preparation method | |
| CN107064256A (en) | A kind of preparation method of naringenin molecular imprinting electrochemical sensor | |
| Shen et al. | Surface modification of activated carbon fiber and its adsorption for vitamin B1 and folic acid | |
| JP2021178850A (en) | Health food and cosmetics for increasing the amount of apoptosis cells and decreasing the amount of necrosis cells and method of manufacturing sprout-forcing grape seed-derived ingredient for increasing the amount of apoptosis cells and decreasing the amount of necrosis cells | |
| CN112206174A (en) | Hydrogenated carbon nanotube gel, preparation method thereof and skin care product | |
| WO2023015824A1 (en) | Electrochemical sensor and preparation method therefor and use thereof in detecting ginsenoside rg3 | |
| CN116554272B (en) | Anti-wrinkle hexapeptide compound and preparation method thereof | |
| CN111568806B (en) | Essential oil-loaded biological polysaccharide and protein modified boron nitride and preparation method and application thereof | |
| Albashari et al. | Local Spinal Cord Injury Treatment Using a Dental Pulp Stem Cell Encapsulated H2S Releasing Multifunctional Injectable Hydrogel | |
| CN108845010A (en) | Ionic liquid auxiliary synthesis of carbon/molybdenum disulfide and graphene oxide composite material are for detecting chloramphenicol | |
| EP1817348B1 (en) | Per-6-guanidino-, -aminoalkylamino-and -guanidino-alkylamino-cyclodextrins, methods of their synthesis and their use for the compaction of dna and intracellular delivery | |
| C Oliveira et al. | Characterization of carbon nanotubes paste electrode and its application as rutin sensor | |
| US4473585A (en) | Method of protecting an object against the attack of destructive fungi employing perdeuteriated N-hendecanoic acid or 2,2-dideutero-N-hendecanoic acid | |
| CN103911680A (en) | Composite collagen fiber and preparation method thereof | |
| CN115671007A (en) | Rhodiola rosea glabridin composite fermentation broth, product containing rhodiola rosea glabridin composite fermentation broth, preparation method and application of rhodiola rosea glabridin composite fermentation broth | |
| CN116327970A (en) | Preparation and application of active oxygen response super-lubrication nano drug-carrying system | |
| CN115414290A (en) | Traditional Chinese medicine composition with moisturizing, antioxidant and anti-inflammatory effects and preparation and application thereof | |
| CN117045547A (en) | Preparation method and application of antioxidant compact supermolecule composite tea fermentation extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210112 |
|
| WD01 | Invention patent application deemed withdrawn after publication |