CN106542575B - A kind of preparation method of nano titanium oxide/nano zinc oxide composite powder material - Google Patents

A kind of preparation method of nano titanium oxide/nano zinc oxide composite powder material Download PDF

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Publication number
CN106542575B
CN106542575B CN201610929040.3A CN201610929040A CN106542575B CN 106542575 B CN106542575 B CN 106542575B CN 201610929040 A CN201610929040 A CN 201610929040A CN 106542575 B CN106542575 B CN 106542575B
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nano
titanium oxide
mixed solution
nano titanium
composite granule
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CN106542575A (en
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杨阳
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SUZHOU YUANLUE INTELLECTUAL PROPERTY OPERATION Co.,Ltd.
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Suzhou Yuxi New Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/08Drying; Calcining ; After treatment of titanium oxide
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27Zinc; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier 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
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/02Oxides; Hydroxides
    • C01G9/03Processes of production using dry methods, e.g. vapour phase processes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/413Nanosized, i.e. having sizes below 100 nm

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Dermatology (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Cosmetics (AREA)

Abstract

The invention belongs to technical field of nano material, and in particular to a kind of preparation method of nano titanium oxide/nano zinc oxide composite powder material, it includes step:Step 1):Zinc acetate and butyl titanate are dissolved in absolute ethyl alcohol, stirred, mixed solution is made;Step 2):By step 1)Water bath method is carried out in obtained mixed solution, is then put in baking oven and is dried, places into and high-temperature roasting is carried out in Muffle furnace, composite granule is made;Step 3):By step 2)Obtained composite granule and stearic acid, carboxymethyl cellulose, hexamethylene mixing and ball milling 1~3 hour.After the present invention organically combines nano zine oxide and nano titanium oxide, the UVA and UVB in solar ultraviolet can be effectively shielded.

Description

A kind of preparation method of nano titanium oxide/nano zinc oxide composite powder material
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of nano titanium oxide/nano zinc oxide compound powder The preparation method of body material.
Background technology
The ultraviolet that solar radiation comes out can be divided into by its wavelength:Wavelength is 320~400nm long wave ultraviolet UVA, the short wave ultraviolet UVC that the ultraviolet B radiation UVB and wavelength that wavelength is 290~320nm are 200~290nm.Research knot Fruit shows:Although fierce reaction will not be caused as UVB by accounting for the UVA of solar ultraviolet 91%, penetration is strong, its 35~ 50% can reach corium, make the fibr tissue of intradermal injured, cause shouting pain, cutis laxa and tanned, be to cause skin photoage And one of the main reason for cutaneum carcinoma.UVC due to having been absorbed substantially in air outer layer.
Nano zine oxide and nano titanium oxide are two kinds of important and widely used inorganic UV sun-screening agents, but its is right UVA and UVB screening ability is discrepant, and nano titanium oxide barrier UVB effect is very good, but the shielding effect to UVA Fruit is not good enough;Nano zine oxide is undesirable to UVB shield effectiveness, but it obstructs UVA effects and is better than nano titanium oxide.
In order to effectively obstruct UVA and UVB, reach overall protected purpose, needed for this comprehensive in sun care preparations Close the characteristic using nano zine oxide and nano titanium oxide.Therefore, how to design one kind and have nano titanium oxide and nanometer concurrently The composite powder material of zinc oxide advantage is study hotspot.
The content of the invention
It is an object of the invention to provide a kind of preparation side of nano titanium oxide/nano zinc oxide composite powder material Method.
In order to realize the purpose of the present invention, the technical solution adopted by the present invention is as follows:
A kind of preparation method of nano titanium oxide/nano zinc oxide composite powder material, it is as follows that it includes step:
Step 1):Zinc acetate and butyl titanate are dissolved in absolute ethyl alcohol, stirred, mixed solution is made;
Step 2):By step 1)Water bath method is carried out in obtained mixed solution, is then put in baking oven and is dried, then It is put into Muffle furnace and carries out high-temperature roasting, composite granule is made;
Step 3):By step 2)Obtained composite granule and stearic acid, carboxymethyl cellulose, hexamethylene mixing and ball milling 1~3 Hour.
Preferably, step 1)In, the amount ratio of the material of described zinc acetate and butyl titanate is 1:(1~3), described vinegar The mass volume ratio 1g of sour zinc and absolute ethyl alcohol:10mL.
Preferably, step 2)In, the high-temperature roasting condition is:Under excess oxygen, 500 DEG C are warming up to 5 DEG C/min Roasting 1~3 hour.
Preferably, step 3)In, described composite granule and stearic acid, carboxymethyl cellulose, the quality volume of cyclohexane Than for 1g:(0.5~0.8)g:(0.05~0.1)g:(5~10)mL.
Compared with prior art, the advantageous effects of technical solution of the present invention are:
1st, nano zine oxide/nano titanium oxide composite powder material preparation method of the invention, nano titanium oxide and The UVA and UVB in solar ultraviolet can be effectively shielded after the combination of nano zine oxide.
2nd, nano zine oxide/nano titanium oxide composite powder material prepared by the present invention, it is fine through stearic acid, carboxymethyl The ball-milling reaction of element is tieed up, changes the surface nature of composite powder material, nano zine oxide/nano titanium oxide composite granule material Material has preferably dispersive property.
3rd, raw material of the invention is easy to get, and cost is low, and reaction is easily controlled.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
1)Weigh 18.35g zinc acetates and 34.03g butyl titanates are dissolved in 183.5mL absolute ethyl alcohols, stir, be made Mixed solution.
2)By mixed solution at 80 DEG C water bath method, be then put in baking oven and be dried, place into Muffle furnace, Under excess oxygen, it is warming up to 500 DEG C with 5 DEG C/min and is calcined 2 hours, composite granule is made.
3)5g composite granules and 3g stearic acid, 0.04g carboxymethyl celluloses, 40mL cyclohexanes mixing and ball milling 2 hours are weighed, .
Embodiment 2
1)Weigh 18.35g zinc acetates and 34.03g butyl titanates are dissolved in 183.5mL absolute ethyl alcohols, stir, be made Mixed solution.
2)By mixed solution at 65 DEG C water bath method, be then put in baking oven and be dried, place into Muffle furnace, Under excess oxygen, it is warming up to 500 DEG C with 5 DEG C/min and is calcined 1 hour, composite granule is made.
3)Weigh 5g composite granules and 2.5g stearic acid, 0.25g carboxymethyl celluloses, 25mL cyclohexanes mixing and ball milling 1 are small When, you can.
Embodiment 3
1)Weigh 18.35g zinc acetates and 34.03g butyl titanates are dissolved in 183.5mL absolute ethyl alcohols, stir, be made Mixed solution.
2)By mixed solution at 95 DEG C water bath method, be then put in baking oven and be dried, place into Muffle furnace, Under excess oxygen, it is warming up to 500 DEG C with 5 DEG C/min and is calcined 3 hours, composite granule is made.
3)5g composite granules and 4g stearic acid, 0.5g carboxymethyl celluloses, 50mL cyclohexanes mixing and ball milling 3 hours are weighed, .
Embodiment 4
Nano titanium oxide made from step 1~3/nano zinc oxide composite powder material is subjected to average grain diameter and printing opacity The test of rate.Wherein, T308 represents transmitance at 308nm, and reflection is screening ability of the composite granule to UVB, T308 Be worth it is smaller, illustrate shield UVB abilities it is better;T360 represents transmitance at 360nm, and reflection is composite granule to UVA Screening ability, T360 values are smaller, illustrate that shielding UVA abilities are better.Test result shows that the average grain diameter of composite granule exists 100nm, T308 value are that 0, T360 values are not more than 2.Nano titanium oxide made from the inventive method-zinc oxide composite powder material Particle mean size is small, strong to UVA and UVB absorbability.

Claims (1)

  1. A kind of 1. preparation method of nano titanium oxide/nano zinc oxide composite powder material, it is characterised in that:Walked including preparing It is rapid as follows:
    Step 1):Zinc acetate and butyl titanate are dissolved in absolute ethyl alcohol, stirred, mixed solution is made;
    Step 2):By step 1)Obtained mixed solution carries out water bath method, is then put in baking oven and is dried, places into horse High-temperature roasting is not carried out in stove, composite granule is made;
    Step 3):By step 2)Obtained composite granule and stearic acid, carboxymethyl cellulose, hexamethylene mixing and ball milling 1~3 are small When;
    Wherein, step 1)In, the amount ratio of the material of described zinc acetate and butyl titanate is 1:(1~3), described zinc acetate with The mass volume ratio 1g of absolute ethyl alcohol:10mL;
    Step 2)In, the high-temperature roasting condition is:Under excess oxygen, it is small to be warming up to 500 DEG C of roastings 1~3 with 5 DEG C/min When;
    Step 3)In, described composite granule is 1g with stearic acid, carboxymethyl cellulose, the mass volume ratio of cyclohexane:(0.5 ~0.8)g:(0.05~0.1)g:(5~10)mL.
CN201610929040.3A 2016-10-31 2016-10-31 A kind of preparation method of nano titanium oxide/nano zinc oxide composite powder material Active CN106542575B (en)

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CN110184596A (en) * 2019-06-20 2019-08-30 佛山市众之助新材料科技有限公司 A method of black phosphating film is covered in metal surface
CN116082893A (en) * 2022-12-29 2023-05-09 广东涂百年新型材料有限公司 Antibacterial dry powder coating and construction method thereof

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