CN117426993A - Reverse-wrapped sun-screening material and preparation method thereof - Google Patents
Reverse-wrapped sun-screening material and preparation method thereof Download PDFInfo
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- CN117426993A CN117426993A CN202311392810.1A CN202311392810A CN117426993A CN 117426993 A CN117426993 A CN 117426993A CN 202311392810 A CN202311392810 A CN 202311392810A CN 117426993 A CN117426993 A CN 117426993A
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- titanium dioxide
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- sun
- nano titanium
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- 239000000463 material Substances 0.000 title claims abstract description 106
- 238000012216 screening Methods 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title abstract description 29
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 107
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000000516 sunscreening agent Substances 0.000 claims abstract description 45
- 239000011787 zinc oxide Substances 0.000 claims abstract description 37
- GYDYJUYZBRGMCC-INIZCTEOSA-N (2s)-2-amino-6-(dodecanoylamino)hexanoic acid Chemical compound CCCCCCCCCCCC(=O)NCCCC[C@H](N)C(O)=O GYDYJUYZBRGMCC-INIZCTEOSA-N 0.000 claims abstract description 32
- 230000000475 sunscreen effect Effects 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract 2
- 239000000725 suspension Substances 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 30
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 23
- 125000002091 cationic group Chemical group 0.000 claims description 20
- 229920002401 polyacrylamide Polymers 0.000 claims description 20
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 20
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 20
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 20
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 20
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 20
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 20
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000002715 modification method Methods 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000037072 sun protection Effects 0.000 abstract description 17
- 239000002245 particle Substances 0.000 description 27
- 239000000758 substrate Substances 0.000 description 19
- 238000000151 deposition Methods 0.000 description 17
- 230000008021 deposition Effects 0.000 description 16
- 230000000694 effects Effects 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 239000006071 cream Substances 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 9
- -1 polydimethylsiloxane Polymers 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 210000004243 sweat Anatomy 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
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- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 3
- 230000002087 whitening effect Effects 0.000 description 3
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 description 2
- ANZUDYZHSVGBRF-UHFFFAOYSA-N 3-ethylnonane-1,2,3-triol Chemical compound CCCCCCC(O)(CC)C(O)CO ANZUDYZHSVGBRF-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229920006037 cross link polymer Polymers 0.000 description 2
- 229940096810 diethylhexyl sebacate Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229920002674 hyaluronan Polymers 0.000 description 2
- 229960003160 hyaluronic acid Drugs 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 125000002347 octyl 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])[H] 0.000 description 2
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 2
- 229960003493 octyltriethoxysilane Drugs 0.000 description 2
- 229960005323 phenoxyethanol Drugs 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000035900 sweating Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 240000008669 Hedera helix Species 0.000 description 1
- 241000196322 Marchantia Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- DLINORNFHVEIFE-UHFFFAOYSA-N hydrogen peroxide;zinc Chemical compound [Zn].OO DLINORNFHVEIFE-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000000913 palmityl 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])([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 1
- 239000011814 protection agent Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- UUJLHYCIMQOUKC-UHFFFAOYSA-N trimethyl-[oxo(trimethylsilylperoxy)silyl]peroxysilane Chemical compound C[Si](C)(C)OO[Si](=O)OO[Si](C)(C)C UUJLHYCIMQOUKC-UHFFFAOYSA-N 0.000 description 1
- 210000001835 viscera Anatomy 0.000 description 1
Classifications
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- 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
-
- 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
- A61K8/24—Phosphorous; 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; 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
- A61K8/19—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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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- 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
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8158—Homopolymers or copolymers of amides or imides, e.g. (meth) acrylamide; Compositions of derivatives of such polymers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- 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
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/817—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
- A61K8/8176—Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
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- 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
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
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- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/596—Mixtures of surface active compounds
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)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to the field of sun protection, and particularly discloses a reverse-wrapped sun protection material and a preparation method thereof. A method of preparing a reverse-encapsulated sunscreen material comprising the steps of: step 1, reacting nano titanium dioxide with lauroyl lysine, performing ultrasonic dispersion, and drying to obtain a heavy reverse wrapping material; and 2, reacting the nano zinc oxide with a heavy reverse wrapping material, performing ultrasonic dispersion, and drying to obtain the double reverse wrapping material. The sun-screening material has the advantages of safety and high-efficiency sun screening; in addition, the preparation method of the invention has the advantages of simple preparation and easy mass production.
Description
Technical Field
The invention relates to the field of sun protection, in particular to a reverse-wrapped sun protection material and a preparation method thereof.
Background
The sun screening material is a material which can absorb ultraviolet light or reflect and diffuse ultraviolet light and can play a role of shielding ultraviolet light, and is often used as a main sun screening component of a sun screening agent.
Traditional sun protection materials are titanium dioxide and zinc oxide. The titanium dioxide has stable chemical property, strong thermal stability and strong hydrophilicity, and has strong absorption capacity for short-wave ultraviolet rays; the zinc oxide has stable chemical property, good dispersivity and good shielding capability on long-wave ultraviolet rays. Thus, titanium dioxide and zinc oxide are commonly added to sun protection products to achieve a broad spectrum sun protection effect. However, the particle sizes of the titanium dioxide and the zinc oxide are large, so that the sun-screening product is easily unevenly distributed when being smeared on the skin surface to generate a pseudo-white effect, and the sun-screening effect and the use experience of the sun-screening cream are affected.
Therefore, the nanoscale titanium dioxide and zinc oxide with smaller particle sizes are widely applied to the sun-screening field due to the advantages of easy smearing, easy dispersion, no false white and the like. At the same time, however, the nano-sized sunscreen materials have small particle sizes, are easy to inhale into the lungs during use, even cause inflammation, and are forbidden to be applied to the field of children sun protection. Thus, there is still room for improvement.
Disclosure of Invention
In order to ensure that the sun-screening material has the effects of safety, high-efficiency sun screening and better use experience, the application provides a reverse-wrapped sun-screening material and a preparation method thereof.
In a first aspect, the present application provides a method for preparing a reverse-wrapped sunscreen material, which adopts the following technical scheme:
step 1, preparing a heavy reverse wrapping material, which comprises the following steps:
step 1-1, respectively dispersing nano titanium dioxide and lauroyl lysine in an organic solvent to form nano titanium dioxide suspension and month Gui Xianlai amino acid suspension;
step 1-2, injecting the nano titanium dioxide suspension into lauroyl lysine suspension, stirring at a constant speed to form a premixed solution, and performing ultrasonic dispersion and drying to obtain a heavy reverse wrapping material;
step 2, preparing a double reverse wrapping material, which comprises the following steps:
step 2-1, respectively dispersing nano zinc oxide and a heavy reverse wrapping material in an organic solvent to form nano zinc oxide suspension and a heavy reverse wrapping material suspension;
and 2-2, injecting the nano zinc oxide suspension into a heavy reverse wrapping material suspension, uniformly stirring to obtain a mixed solution, and performing ultrasonic dispersion and drying to obtain the double reverse wrapping material.
By taking lauroyl lysine of a lamellar structure as a base substrate, nano titanium dioxide is firstly deposited on the basis of lauroyl lysine, and then nano zinc oxide is secondarily deposited, so that a laminated lamellar structure with front and back surfaces, namely a sandwich-like structure model, is formed, nano titanium dioxide and nano zinc oxide powder are firmly adhered to the micron-sized base substrate, the ultraviolet resistance effect of nano titanium dioxide and zinc oxide can be achieved, the safety of nano level is achieved, and the inhalation risk is not easy to exist. Meanwhile, the reverse wrapping laminated sheet structure has larger surface area, so that the sun-screening agent can better absorb and scatter ultraviolet rays when being smeared on skin, and further, the sun-screening effect is better improved; the base substrate has smooth surface and uniform particle size, and after being reversely wrapped by nano titanium dioxide and zinc oxide, a more uniform and compact wrapping layer is formed, so that the sun-screening agent has more excellent adhesion, softer skin-lubricating feel like silk, and more uniform contact between the sun-screening agent and skin, thereby being beneficial to further improving the transparency and stability of the sun-screening agent and reducing the phenomena of false white and layering of sun-screening products; after being subjected to lamination and wrapping treatment, the sun-screening agent is better protected, and the contact reaction of the sun-screening agent and other chemical substances is reduced, so that the sun-screening agent has higher stability, better hydrophobicity and better resistance to sweat, water and friction, and further longer-lasting sun-screening is better realized; in addition, the nano-sunscreen agent after being packaged is beneficial to further reducing the astringent feeling, thereby being beneficial to reducing the deposition of particles on the skin.
Preferably, the nano titanium dioxide is modified nano titanium dioxide, and the modification method of the nano titanium dioxide is as follows: titanium dioxide, sodium hexametaphosphate, cationic polyacrylamide, polyvinylpyrrolidone and deionized water (40-50): (0.1-0.4): (0.03-0.07): (0.03-0.07): mixing the materials (500-1000) in a mass ratio to prepare a suspension, placing the suspension in a constant-temperature water tank with the temperature of 50-70 ℃, slowly dripping 50-60mL of aluminum chloride solution with the mass concentration of 40-50g/L into the suspension, continuously dripping sodium hydroxide solution at the same time to keep the pH of the suspension at 5.5-6.0 all the time, continuously dripping sodium hydroxide solution until the addition of the aluminum chloride solution is completed, regulating the pH of the suspension to 6.5-7.5, washing and drying to obtain the modified nano titanium dioxide.
By adopting the method to modify the nano titanium dioxide, the surface of the nano titanium dioxide is uniformly coated with the hydrated alumina gel to form an electric double layer, which is beneficial to improving the compatibility of the modified nano titanium dioxide and lauroyl lysine and enabling the nano titanium dioxide to be uniformly coated on the surface of the lauroyl lysine; meanwhile, three surfactants of sodium hexametaphosphate, cationic polyacrylamide and polyvinylpyrrolidone are adopted for synergistic compounding, so that ionization of anions and cations is facilitated, the concentration of the anions and the cations in a solution is improved, an electric double layer of hydrated alumina gel is compressed, the tendency of gel to separate from a water phase is increased, the deposition degree of modified nano titanium dioxide on the surface of lauroyl lysine is improved, meanwhile, the dispersibility is not easily reduced due to the too high deposition degree, the particle size of a sun-screening material is too large, and the use experience of the sun-screening material is affected; the method is also beneficial to improving the hydrophobicity of the sun cream, is not easy to cause floating powder to make up and reduce the durability of the sun cream.
Preferably, the mass ratio of the titanium dioxide, the sodium hexametaphosphate, the cationic polyacrylamide, the polyvinylpyrrolidone and the deionized water is as follows: (44-46): (0.2-0.3): (0.05-0.06): (0.05-0.06): (700-800); the mass concentration of the aluminum chloride solution is 43-47g/L.
By adopting the specific substances and the specific mass ratio, the deposition degree of the modified nano titanium dioxide is improved, and meanwhile, the particle size of the sun-proof material is overlarge and the use experience is influenced because the deposition degree of the nano titanium dioxide on the surface of the substrate is too high and the dispersibility is reduced.
Preferably, the temperature of the constant temperature water tank is 55-65 ℃.
By adopting the specific water bath temperature, the dispersibility of the nano titanium dioxide in the deionized water is improved, and the deposition degree of the nano titanium dioxide on the surface of the substrate is reduced due to the overhigh dispersibility, so that the sun-proof performance of the sun-proof cream is affected.
Preferably, the mass concentration of the nano titanium dioxide is 1-10g/L; the mass concentration of lauroyl lysine is 1-2g/L; the mass concentration of the heavy reverse wrapping material is 2-6g/L; the mass concentration of the nano titanium dioxide is 1-10g/L.
The suspension liquid with specific mass concentration is added, so that the deposition degree of the nano titanium dioxide on the surface of the substrate is improved, meanwhile, the dispersibility of the nano titanium dioxide on the surface of the substrate is not easy to be reduced due to overhigh deposition, the particle size of the sun-proof material is overlarge, and the use experience is affected.
Preferably, the stirring time is 10-30 minutes; the stirring speed is 200-400r/min; the ultrasonic dispersion time is 10-20 minutes.
By adopting specific stirring time, stirring speed and ultrasonic dispersion time, the method is favorable for crushing large nano agglomerated particles, improves the dispersibility of the nano material, ensures that the formed sun-screening material has more uniform structure and is favorable for improving the characteristic of easy smearing of the sun-screening material; the nanometer material is not easy to deposit due to low dispersion process, so that the particle size of the sun-proof material is too large, and the use experience is affected.
Preferably, the organic solvent includes one or more of ethanol, methanol, and glycerol.
By adopting the organic solvent, the dispersibility of the nano material is improved, so that the nano material is not easy to excessively deposit on the surface of the substrate, and the particle size of the sun-screening material is overlarge; meanwhile, the health protection agent is not easy to cause harm to human health.
In a second aspect, the present application provides a reverse-wrapped sunscreen material made by the method described above.
The reversely-wrapped sun-screening material prepared by the method is favorable for forming the sun-screening material with a sandwich structure, and realizes broad-spectrum sun-screening of long/short-wave ultraviolet rays; it is also beneficial to form sun-screening material with larger particle size, and reduces the risk of inflammation caused by inhalation into the viscera.
In summary, the present application has the following beneficial effects:
1. by taking lauroyl lysine as a base substrate, sequentially depositing nano titanium dioxide and nano zinc oxide, the reversely-wrapped nano sun-screening material is formed, the broad-spectrum sun-screening effect can be achieved, the nano-level safety is achieved, and the risk of inhalation is not easy to exist. Meanwhile, the nano titanium dioxide is completely coated in the nano zinc oxide by adopting a double coating mode, so that false white is not easy to occur.
2. The nano titanium dioxide is modified by coating the hydrated alumina on the surface, so that the compatibility of the nano titanium dioxide and lauroyl lysine is improved, the nano titanium dioxide is beneficial to forming a uniform and compact coating layer on the surface of the lauroyl lysine, the particle size of the sun-screening material is not easy to be excessively large due to excessive deposition of the nano titanium dioxide, the dispersibility of sun-screening cream is reduced, and the sun-screening material is not easy to be smeared.
Drawings
FIG. 1 is a scanning electron microscope image of the sunscreen material prepared in example 1;
FIG. 2 is a scanning electron microscope image of the larger particle size sunscreen of FIG. 1;
FIG. 3 is a scanning electron microscope image of the sunscreen material prepared in comparative example 1;
FIG. 4 is a scanning electron microscope image of the sunscreen material prepared in comparative example 2;
fig. 5 is a scanning electron microscope image of the larger particle size sunscreen of fig. 4.
Detailed Description
The present application is described in further detail below with reference to examples.
The following examples and comparative examples were all commercially available and were prepared as follows:
lauroyl lysine was purchased from Hubei Fangde New Material Co., ltd;
cationic polyacrylamide was purchased from Shandong Ruihai New Material technologies Co., ltd;
sodium hexametaphosphate was purchased from the state-area Bihai chemical Co., ltd;
cyclopentadimethicone was purchased from Wuhan Xin Wei Di Ji chemical Co., ltd;
polydimethylsiloxane was purchased from Shanghai Seiyaka Biotechnology Co., ltd;
HDI/trihydroxy hexyl lactone crosslinked polymer was purchased from beijing labao technologies limited;
triethoxyoctylsilane is available from Shanghai Seiyaka Biotechnology Co., ltd;
silica is available from Shanghai, inc.;
polyglycerol-6 was purchased from taan Jiang Zhou biotechnology limited;
PEG/PPG-18/18 was purchased from Beijing lablab technologies Co., ltd;
trimethylsilyloxy silicate was purchased from baolong international trade limited in guangzhou;
octyl polymethylsiloxane was purchased from Hubei institute of biotechnology limited;
dimethylsilyl silica is available from Fosman technologies Co., ltd;
ethylhexyl glycerol was purchased from south Beijing Tianshi blue shield biotechnology Co., ltd;
essence was purchased from Jiangxi Hai Rui Natural plant Co., ltd;
aminosilanes were purchased from marchantia and chemical technology limited;
the CAS number of polyvinylpyrrolidone is 88-12-0;
the CAS number of the polyvinyl alcohol is 9002-89-5;
the CAS number of the sodium dodecyl sulfate is 151-21-3;
cetyl trimethyl ammonium bromide has a CAS number of 57-09-0;
the CAS number of the nano zinc oxide is 1314-13-2;
the CAS number of the polydimethylsiloxane is 9016-00-69;
the CAS number of phenoxyethanol is 122-99-6;
the CAS number of the hyaluronic acid is 9004-61-9;
the CAS number of the sodium chloride is 7647-14-5;
the CAS number of the aluminum hydroxide is 21645-51-2;
stearic acid has a CAS number of 57-11-4;
the CAS number for diethyl hexyl sebacate is 122-62-3.
Preparation example 1
The preparation example of the application discloses a modification method of modified nano titanium dioxide, which comprises the following steps:
adding 4.0g of nano titanium dioxide into 50mL of water, and then adding sodium hexametaphosphate with the mass concentration of 10g/L, cationic polyacrylamide with the mass concentration of 3g/L and polyvinylpyrrolidone with the mass concentration of 3g/L into the water, wherein the mass ratio of titanium dioxide, sodium hexametaphosphate, cationic polyacrylamide, polyvinylpyrrolidone and deionized water is 40:0.1:0.03:0.03:500, preparing a suspension, and placing the suspension in a constant-temperature water tank at 50 ℃; 50mL of an aluminum chloride solution with a mass concentration of 40g/L was added to the suspension at a flow rate of 3mL/min, and a sodium hydroxide solution with a mass concentration of 0.1mol/L was added dropwise while the aluminum chloride solution was being added dropwise, so that the pH of the whole system was always kept stable at 5.5. And after 50mL of aluminum chloride solution is completely added into the suspension, finally, continuously using sodium hydroxide with the mass concentration of 0.1mol/L to adjust the pH value of the suspension to 6.5, standing for 90 minutes, filtering by using a funnel, taking a filter cake, washing with water, and drying in an oven with the temperature of 60 ℃ to obtain the modified nano titanium dioxide.
Preparation example 2
The preparation example of the application discloses a modification method of modified nano titanium dioxide, which comprises the following steps:
5.0g of nano titanium dioxide is added into 100mL of water, and sodium hexametaphosphate with the mass concentration of 40g/L, 7g/L of cationic polyacrylamide and 7g/L of polyvinylpyrrolidone are added into the water, wherein the mass ratio of titanium dioxide, sodium hexametaphosphate, cationic polyacrylamide, polyvinylpyrrolidone and deionized water is 50:0.4:0.07:0.07:1000, preparing a suspension, and placing the suspension in a constant temperature water tank at 70 ℃; 60mL of an aluminum chloride solution with a mass concentration of 60g/L was added to the suspension at a flow rate of 5mL/min, and a sodium hydroxide solution with a mass concentration of 0.1mol/L was continuously added dropwise, so that the pH of the whole system was constantly kept at 6.0. After 50mL of aluminum chloride solution is fully added into the suspension, finally, the pH of the suspension is regulated to 7.5 by sodium hydroxide with the mass concentration of 0.1mol/L, the suspension is kept stand for 90 minutes, a funnel is used for filtering, a filter cake is taken and washed by water, and the filter cake is dried in an oven with the temperature of 60 ℃ to obtain the modified nano titanium dioxide.
Preparation example 3
The difference from the preparation example 1 is that: sodium hexametaphosphate was replaced with an equal amount of sodium lauryl sulfate.
Preparation example 4
The difference from the preparation example 1 is that: the cationic polyacrylamide is replaced by equal amount of sodium cetyl trimethyl sulfonate.
Preparation example 5
The difference from the preparation example 1 is that: polyvinyl alcohol was replaced with equal amounts of polyvinyl pyrrolidone.
Preparation example 6
The difference from the preparation example 1 is that: the dosage, mass concentration and addition volume of each component of the modified nano titanium dioxide in the modification process are as follows:
the titanium dioxide dosage is 4.4g; the mass concentration of the sodium hexametaphosphate is 20g/L; the mass concentration of the cationic polyacrylamide is 5g/L; the mass concentration of polyvinylpyrrolidone is 5g/L; the dosage of deionized water is 70g; the mass concentration of the aluminum chloride solution is 43g/L. Wherein, the added volumes of sodium hexametaphosphate, cationic polyacrylamide and polyvinylpyrrolidone are all 0.7mL.
Namely, the mass ratio of titanium dioxide, sodium hexametaphosphate, cationic polyacrylamide, polyvinylpyrrolidone and deionized water is 44:0.2:0.05:0.05:700.
preparation example 7
The difference from example 2 is that: the dosage, mass concentration and addition volume of each component in the modification process of the modified nano titanium dioxide are specifically as follows:
the titanium dioxide dosage is 4.6g; the mass concentration of the sodium hexametaphosphate is 30g/L; the mass concentration of the cationic polyacrylamide is 6g/L; the mass concentration of polyvinylpyrrolidone is 6g/L; the dosage of deionized water is 80g; the mass concentration of the aluminum chloride solution is 47g/L. Wherein, the added volumes of sodium hexametaphosphate, cationic polyacrylamide and polyvinylpyrrolidone are all 0.8mL.
Namely, the mass ratio of titanium dioxide, sodium hexametaphosphate, cationic polyacrylamide, polyvinylpyrrolidone and deionized water is 46:0.3:0.06:0.06:800.
example 1
The embodiment of the application discloses a preparation method of a reverse-wrapped sun-screening material, which comprises the following steps:
step 1, preparing a heavy reverse wrapping material, which comprises the following steps:
step 1-1, adding 5.5g of nano titanium dioxide and 1.5g of lauroyl lysine into 1L of absolute ethyl alcohol respectively, and stirring for 10 minutes at a rotating speed of 100r/min to form a nano titanium dioxide suspension with a mass concentration of 5.5g/L and a month Gui Xianlai amino acid suspension with a mass concentration of 1.5 g/L.
And 1-2, injecting 100mL of nano titanium dioxide suspension into 100mL of lauroyl lysine suspension at a flow rate of 60mL/min, heating to 40 ℃, stirring for 20 minutes at a rotating speed of 300r/min to form a premixed solution, and performing ultrasonic dispersion for 15 minutes by using ultrasonic frequency of 35 KHz. And standing the mixed solution, cooling to room temperature, filtering by using a funnel, and drying the filter cake in an oven at 60 ℃ to obtain the heavy reverse wrapping material.
Step 2, preparing a double reverse wrapping material, which comprises the following steps:
and 2-1, respectively adding 5.5g of nano zinc oxide and 4.0g of a heavy reverse wrapping material into 1L of absolute ethyl alcohol, and stirring at a speed of 100r/min for 10 minutes to form a nano zinc oxide suspension with a mass concentration of 5.5g/L and a suspension of the heavy reverse wrapping material.
And 2-2, injecting 100mL of nano zinc oxide suspension into 100mL of suspension of a heavy reverse wrapping material at a flow rate of 60mL/min, heating to 40 ℃, stirring at a rotating speed of 300r/min for 20 minutes to obtain a mixed solution, and performing ultrasonic dispersion for 15 minutes by using ultrasonic frequency of 35 KHz. And standing the mixed solution to room temperature, filtering by using a funnel, and drying the filter cake in an oven with the temperature of 60 ℃ to obtain the double reverse wrapping material.
Example 2
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 1.
Example 3
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 2.
Example 4
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 3.
Example 5
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 4.
Example 6
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 5.
Example 7
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 6.
Example 8
The difference from example 1 is that:
the nano titanium dioxide is modified nano titanium dioxide, and the modified nano titanium dioxide is prepared in preparation example 7.
Example 9
The difference from example 2 is that: the temperature of the thermostatic water bath was 55 ℃.
Example 10
The difference from example 2 is that: the temperature of the thermostatic water bath was 65 ℃.
Example 11
The difference from example 2 is that:
the mass concentration of the components in the synthesis process of the reversely-wrapped sun-screening material is as follows: lauroyl lysine 1g/L; nano titanium dioxide 1.0g/L; 1.0g/L of nano zinc oxide; a heavy reverse wrapper of 2.0g/L.
The parameters during the synthesis of the reverse-wrap sunscreen material were as follows: the rotating speed is 200r/min; stirring for 10 minutes; ultrasound time 10 minutes.
Example 12
The difference from example 2 is that:
the mass concentration of the components in the synthesis process of the reversely-wrapped sun-screening material is as follows: lauroyl lysine 2g/L; 10g/L of nano titanium dioxide; 10g/L of nano zinc oxide; a heavy reverse wrapper of 6g/L.
The parameters during the synthesis of the reverse-wrap sunscreen material were as follows: the rotating speed is 400r/min; stirring for 30 minutes; ultrasound time was 20 minutes.
Comparative example 1
The comparative example of the present application discloses a method for preparing a sunscreen material, comprising the following steps:
step 1, adding 5.5g of nano titanium dioxide and 5.5g of nano zinc oxide into 1L of absolute ethyl alcohol respectively to form a nano titanium dioxide suspension with the mass concentration of 5.5g/L and a nano zinc oxide suspension with the mass concentration of 5.5 g/L;
and 2, injecting 100mL of nano titanium dioxide suspension into 100mL of nano zinc oxide suspension at a flow rate of 60mL/min, heating to 40 ℃, stirring for 20 minutes at a rotating speed of 300r/min to form a mixed solution, and performing ultrasonic dispersion for 15 minutes. And cooling the mixed solution to room temperature and then drying to obtain the sun-screening material.
Comparative example 2
The comparative example of the present application discloses a method for preparing a sunscreen material, comprising the following steps:
step 1, dispersing 5.5g of nano titanium dioxide, 5.5g of nano zinc oxide and 1.5g of lauroyl lysine in 1L of absolute ethyl alcohol respectively to form a nano titanium dioxide suspension with the mass concentration of 5.5g/L, a nano zinc oxide suspension with the mass concentration of 5.5g/L and a lauroyl lysine suspension with the mass concentration of 1.5 g/L;
and 2, respectively injecting 100mL of nano titanium dioxide suspension and 100mL of nano zinc oxide suspension into 100mL of lauroyl lysine suspension at a flow rate of 60mL/min, heating to 40 ℃, stirring for 20 minutes at a rotation speed of 300r/min to form a mixed solution, and performing ultrasonic dispersion for 15 minutes. And cooling the mixed solution to room temperature and then drying to obtain the sun-screening material.
Experiment 1
The sun-screening materials prepared in the above examples and comparative examples were selected to be 0.2g each, uniformly adhered to a sample stage having a conductive paste, and the magnification of a field emission scanning electron microscope was adjusted to 1000 times, an electron microscope image was taken at this magnification, the morphology of the sun-screening material in the electron microscope image was observed, the particle size range (μm) of the sun-screening material was measured using an analytical tool provided with the apparatus, and the average particle size (μm) of the sun-screening material was calculated. The model of the field emission scanning electron microscope is SEM4000, and the manufacturer is national instrument quantum technology Co.
The above experimental data are detailed in table 1.
Experiment 2
The sun-screening materials prepared in the experimental examples and the comparative examples are selected to prepare sun-screening cream, and the preparation steps are as follows:
step 1, 8.2g of water is taken and injected into a container, 7.0g of octyl polymethylsiloxane, 3.0g of polydimethylsiloxane and 0.5kg of dimethylsilylated silica are added, and the mixture is stirred for 5 minutes at a rotating speed of 100r/min to form a premix for later use;
step 2, 8.2k of water is taken and injected into a container, and polyglycerol-6.0 g, hyaluronic acid 0.1g and sodium chloride 0.4g are added, and stirred for 5 minutes at a rotating speed of 100r/min to form a mixture for standby;
step 3, adding 65g of reverse-wrapped sun-screening material, 3g of cyclopentadimethicone, 3g of PEG/PPG-18/18 g of PEG/PPG-18 g of trimethylsiloxysilicate, 1g of diethyl hexyl sebacate, 1g of HDI/trihydroxyhexyl lactone crosslinked polymer, 0.5g of triethoxyoctyl silane, 0.5g of silica, 0.5g of aluminum hydroxide and 1.0g of stearic acid into a main pot in sequence, and stirring at a speed of 100r/min for 10 minutes; adding the premix, and stirring at a speed of 100r/min for 5 minutes;
and 4, starting stirring, wherein the stirring speed is 150r/min, adding the mixture into a main pot, stirring for 5min, adding 0.2g of phenoxyethanol, 0.2g of ethylhexyl glycerol and 0.2g of essence, and stirring for 5min at a rotating speed of 100 r/min.
Female volunteers with ages 25-35 years old, skin color of cold white and smooth and flawless facial skin were randomly selected 100. Volunteers were equally divided into 20 groups of 5 persons each, and sunscreen creams each using the sunscreen materials prepared by adding the above examples and comparative examples were used. The volunteer takes 0.1g of sun cream and smears the right cheek with a hand slightly, the smearing area is 400mm 2 Observing and counting the use experience of volunteers when the volunteers smear the sun cream; and in two hours after application, volunteers need to sit still at the indoor temperature of 40 ℃ until the cheek has fine sweat beads, and the makeup effect of the sun cream under the condition of sweating is observed.
The above experimental data are detailed in table 1.
Experiment 3
The sun-screening cream prepared by the sun-screening materials prepared in the example and the comparative example in the experiment 2 is taken respectively in an amount of 0.2g, and the sun-screening indexes SPF and PFA of the sun-screening cream are measured by an ultraviolet resistance tester, so that the larger the measured sun-screening index SPF is, the stronger the sun-screening effect is, the higher the sun-screening index PFA is, and the longer the sun-screening time is. Wherein, ultraviolet resistance tester is purchased from Shanghai extensive textile detection technology Co.
Details of the above experimental data are shown in table 1.
TABLE 1
According to the data comparison of the example 1 and the comparative examples 1-2 in the table 1, the example 1 adopts lauroyl lysine as a base substrate, and sequentially covers nano titanium dioxide and nano zinc oxide to synthesize a double-coated sun-screening material, and as shown in fig. 1, the sun-screening materials are all micron-sized spherical or elliptic particles; as shown in fig. 2, the sunscreen material prepared by double wrapping was smooth in surface. Wherein, the nano titanium dioxide is coated in the nano zinc oxide, so that the false white effect is not easy to occur; meanwhile, the double-coated sun-screening material is synthesized by sequentially covering the nano titanium dioxide and the nano zinc oxide, the sun-screening cream has strong capability of absorbing and scattering long/short wave ultraviolet rays, and a broad-spectrum sun-screening effect can be realized. In comparative example 1, the sun-screening material formed by directly mixing nano titanium dioxide and nano zinc oxide is not easy to agglomerate, as shown in fig. 3, no obvious sun-screening material in a particle shape is found in the figure; meanwhile, the nano zinc oxide cannot completely cover the nano titanium dioxide, so that the sun cream has a pseudo-white effect and has poor sun protection effect. Comparative example 2 a sunscreen material prepared by using lauroyl lysine as a substrate and simultaneously adding nano titanium dioxide and nano zinc oxide to coat the surface of the substrate, wherein the formed sunscreen material is in a granular shape as shown in fig. 4; as shown in fig. 5, compared with example 1, there is only one encapsulation process, and the unmodified nano zinc dioxide is not well compatible with lauroyl lysine, resulting in a sun-screening material with a lower surface smoothness and a slightly lower average particle size than example 1; meanwhile, the nano titanium dioxide cannot be completely coated, so that false white is easy to appear, and the sun-proof effect is poor. Proved by the prior art, the broad-spectrum sun protection can be realized by adopting the mode of taking lauroyl lysine as a substrate and sequentially coating nano titanium dioxide and nano zinc oxide to prepare the sun protection material, and meanwhile, the particle size of the sun protection material is improved, and the safety of sun protection cream is enhanced.
According to the data comparison of examples 1-3 in Table 1, the sunscreen cream prepared by adopting the unmodified nano titanium dioxide in example 1 has higher sun protection index, can be easily smeared by volunteers when in use, has uniform texture and no false white, and has no conditions of floating powder and whitening when the volunteers sweat. In the embodiment 2-3, the modified nano titanium dioxide is used, the hydrated alumina gel coated on the surface of the modified nano titanium dioxide has a large tendency to separate from the water phase, has strong hydrophobicity, improves the compatibility of the nano titanium dioxide on the surface of a substrate, ensures that the nano titanium dioxide is uniformly coated on the surface of lauroyl lysine, and further improves the sun-screening effect of the sun-screening material; meanwhile, the prepared sun cream has higher hydrophobicity, sweat is not easy to fall off, and the phenomena of floating powder and whitening are not easy to occur. The modified nano titanium dioxide is proved to be beneficial to improving the compatibility of the nano titanium dioxide and lauroyl lysine, so that the nano titanium dioxide is uniformly coated on the surface of the lauroyl lysine, and the sun protection index of the sun protection material is further improved.
According to the data comparison of examples 3-6 in Table 1, sodium hexametaphosphate, cationic polyacrylamide and polyvinylpyrrolidone are added in example 3, and the prepared sun cream has higher sun protection index, can be easily smeared by volunteers when used, has uniform texture, is not false white, and does not generate the conditions of floating powder and whitening during perspiration; in the examples 4-6, sodium dodecyl sulfate, sodium hexadecyl trimethyl sulfonate and polyvinyl alcohol are respectively used for replacing sodium hexametaphosphate, cationic polyacrylamide and polyvinylpyrrolidone to prepare modified nano titanium dioxide, the hydrated alumina gel coated on the surface of the modified nano titanium dioxide has small tendency to separate from a water phase and poor hydrophobicity, the deposition degree of the modified nano titanium dioxide on the surface of a substrate is too high, the dispersibility is reduced, and the particle size of the sun-screening material is increased; meanwhile, the prepared sun cream has reduced hydrophobicity, is easy to whiten and fall off during sweating, and has poor makeup holding effect. The modified nano titanium dioxide is prepared by adding three surfactants of sodium hexametaphosphate, cationic polyacrylamide and polyvinylpyrrolidone to be compounded in a synergistic way, so that the deposition degree of the modified nano titanium dioxide on lauroyl lysine can be improved, and meanwhile, the dispersity is reduced due to the fact that the deposition degree of the modified nano titanium dioxide on the surface of lauroyl lysine is too high, the particle size of a sun-screening material is too large, and the use experience of the sun-screening material is affected.
According to the data comparison of the embodiment 1 and the embodiments 7-8 in the table 1, the suspension liquid with specific mass concentration is adopted to modify the nano titanium dioxide, so that the deposition degree of the nano titanium dioxide on the surface of the substrate is improved, meanwhile, the dispersibility of the nano titanium dioxide on the surface of the substrate is not easy to be reduced due to the too high deposition, the particle size of the sun-screening material is too large, and the use experience is affected.
According to the data comparison of the embodiment 1 and the embodiment 9-10 in the table 1, by adopting the proper temperature, the dispersibility of the nano material in deionized water is improved, the reaction rate is improved, the structure of the sun-screening material is more uniform, and the use experience is better; the structure of the sun-screening material is more uniform, and the sun-screening performance of the material is improved.
According to the data comparison of the embodiment 1 and the embodiments 11-12 in the table 1, the suspension liquid with specific mass concentration is adopted to modify the nano titanium dioxide, so that the deposition degree of the nano titanium dioxide on the surface of the substrate is improved, meanwhile, the dispersibility of the nano titanium dioxide on the surface of the substrate is not easy to be reduced due to the excessively high deposition, the particle size of the sun-screening material is excessively large, and the use experience is affected. By adopting specific stirring time, stirring speed and ultrasonic dispersion time, the method is favorable for crushing large nano agglomerated particles, improves the dispersibility of the nano material, ensures that the formed sun-screening material has more uniform structure and is favorable for improving the characteristic of easy smearing of the sun-screening material; the nanometer material is not easy to deposit due to low dispersion process, so that the particle size of the sun-proof material is too large, and the use experience is affected.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. A method for preparing a reverse-wrapped sun-screening material, which is characterized by comprising the following steps: the method comprises the following steps:
step 1, preparing a heavy reverse wrapping material, which comprises the following steps:
step 1-1, respectively dispersing nano titanium dioxide and lauroyl lysine in an organic solvent to form nano titanium dioxide suspension and month Gui Xianlai amino acid suspension;
step 1-2, injecting the nano titanium dioxide suspension into lauroyl lysine suspension, stirring to form a premixed solution, and then performing ultrasonic dispersion and drying to obtain a heavy reverse wrapping material;
step 2, preparing a double reverse wrapping material, which comprises the following steps:
step 2-1, respectively dispersing nano zinc oxide and a heavy reverse wrapping material in an organic solvent to form nano zinc oxide suspension and a heavy reverse wrapping material suspension;
and 2-2, injecting the nano zinc oxide suspension into a heavy reverse wrapping material suspension, stirring to obtain a mixed solution, and performing ultrasonic dispersion and drying to obtain the double reverse wrapping material.
2. A method of preparing a reverse-encapsulated sunscreen according to claim 1, wherein: the nano titanium dioxide is modified nano titanium dioxide, and the modification method of the nano titanium dioxide comprises the following steps:
titanium dioxide, sodium hexametaphosphate, cationic polyacrylamide, polyvinylpyrrolidone and deionized water (40-50): (0.1-0.4): (0.03-0.07): (0.03-0.07): mixing the materials (500-1000) in a mass ratio to prepare a suspension, placing the suspension in a constant-temperature water tank with the temperature of 50-70 ℃, then dripping 50-60mL of aluminum chloride solution with the mass concentration of 40-50g/L into the suspension, continuously dripping sodium hydroxide solution at the same time to keep the pH of the suspension at 5.5-6.0 all the time, continuously dripping sodium hydroxide solution after the addition of the aluminum chloride solution is finished, adjusting the pH of the suspension to 6.5-7.5, washing and drying to obtain the modified nano titanium dioxide.
3. A method of preparing a reverse-encapsulated sunscreen according to claim 2, wherein: the mass ratio of the titanium dioxide, the sodium hexametaphosphate, the cationic polyacrylamide, the polyvinylpyrrolidone and the deionized water is as follows: (44-46): (0.2-0.3): (0.05-0.06): (0.05-0.06): (700-800); the mass concentration of the aluminum chloride solution is 43-47g/L.
4. A method of preparing a reverse-encapsulated sunscreen according to claim 2, wherein: the temperature of the constant temperature water tank is 55-65 ℃.
5. A method of preparing a reverse-encapsulated sunscreen according to claim 1, wherein: in the step 1-1, the mass concentration of the lauroyl lysine suspension is 1-2g/L; the mass concentration of the nano titanium dioxide suspension is 1-10g/L; in the step 2-1, the mass concentration of the nano zinc oxide suspension is 1-10g/L; the mass concentration of the heavy reverse wrapping material suspension is 2-6g/L.
6. A method of preparing a reverse-encapsulated sunscreen according to claim 1, wherein: in the step 1-2 and the step 2-2, the stirring speed is 200-400r/min; stirring for 10-30 min; the ultrasonic time is 10-20 minutes.
7. A method of preparing a reverse-encapsulated sunscreen according to claim 1, wherein: the organic solvent comprises one or more of ethanol, methanol and glycerol.
8. A reverse-wrapped sunscreen material characterized by: a method of making a reverse-encapsulated sunscreen material as claimed in any one of claims 1 to 7.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311392810.1A CN117426993A (en) | 2023-10-25 | 2023-10-25 | Reverse-wrapped sun-screening material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311392810.1A CN117426993A (en) | 2023-10-25 | 2023-10-25 | Reverse-wrapped sun-screening material and preparation method thereof |
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| CN117426993A true CN117426993A (en) | 2024-01-23 |
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| CN202311392810.1A Pending CN117426993A (en) | 2023-10-25 | 2023-10-25 | Reverse-wrapped sun-screening material and preparation method thereof |
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