CN110314676A - The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application - Google Patents

The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application Download PDF

Info

Publication number
CN110314676A
CN110314676A CN201910669234.8A CN201910669234A CN110314676A CN 110314676 A CN110314676 A CN 110314676A CN 201910669234 A CN201910669234 A CN 201910669234A CN 110314676 A CN110314676 A CN 110314676A
Authority
CN
China
Prior art keywords
powder
nano
tio
water
acetic acid
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
Application number
CN201910669234.8A
Other languages
Chinese (zh)
Inventor
李佳颖
刘世民
赵东扬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian Jiaotong University
Original Assignee
Dalian Jiaotong University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Dalian Jiaotong University filed Critical Dalian Jiaotong University
Priority to CN201910669234.8A priority Critical patent/CN110314676A/en
Publication of CN110314676A publication Critical patent/CN110314676A/en
Pending legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/391—Physical properties of the active metal ingredient
    • B01J35/393—Metal or metal oxide crystallite size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/10—Heat treatment in the presence of water, e.g. steam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/12—Oxidising
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
    • C09D5/1612—Non-macromolecular compounds
    • C09D5/1618—Non-macromolecular compounds inorganic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/06—Polluted air
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Nanotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing & Machinery (AREA)
  • Water Supply & Treatment (AREA)
  • Toxicology (AREA)
  • Composite Materials (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Detergent Compositions (AREA)

Abstract

The present invention relates to nano material production technical fields more particularly to a kind of direct solution oxide method preparation Sn of high water to adulterate TiO2Nano-powder and its application use H using stannic chloride pentahydrate and butyl titanate as presoma2For O as solvent, glacial acetic acid is stabilizer, and the 0.5at%Sn doping TiO of the good different waters of crystallinity height, photocatalysis performance is prepared at 70-150 DEG C2Nano-powder, average grain diameter 2-7nm.150 times of H at 150 DEG C are taken in experiment respectively2The Sn of O adulterates TiO2Nano-powder and undoped TiO2Nano-powder 10g, 200mL deionized water grinds 10min after 0.05mL dispersing agent (acrylic acid dispersant) mixing, spray is made and is sprayed on degradation of formaldehyde on wallpaper, the former works well.The Sn of this high direct solution oxide method preparation of water adulterates TiO2Nano-powder has many advantages, such as high catalytic activity, stable chemical performance, nontoxic, pollution-free, nonirritant, heat-resist, low in cost, can be applied to the fields such as sewage treatment, air cleaning, antibacterial and deodouring, antifouling self-cleaning glass.

Description

The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application
Technical field
The present invention relates to nano material production technical fields more particularly to a kind of direct solution oxide method of high water to prepare Sn Adulterate TiO2Nano-powder and its application.
Background technique
TiO2It is widely used in cosmetics, fine ceramics, coating, sewage treatment, photocell etc., and has nothing The advantages that poison, spectrochemical property are stable, oxidability is strong, in fields such as photocatalysis, antibacterial and organic pollutant degradations by pass Note.And pure TiO on the market2Nano material generally will could obtain crystal property and light by 300 DEG C or more high-temperature calcinations The good TiO of catalytic performance2Nano material, and TiO obtained by high temperature2Crystal form and partial size have baneful influence to its photocatalysis performance. Therefore, TiO is improved2The trend that the photocatalytic activity of nano material is studied at present.
Summary of the invention
The purpose of the invention is to prepare crystal property and the good 0.5at%Sn of photocatalysis performance to adulterate TiO2It receives Rice flour body, the present invention are directed under conventional high-temperature (300 DEG C or more) and prepare TiO2The defect of nano-powder, it is directly molten using high water Liquid oxidation method uses water to replace ethyl alcohol as solvent using butyl titanate and stannic chloride pentahydrate as raw material, and glacial acetic acid is stabilizer, Instead of traditional sol-gal process, variation (butyl titanate (CP), H of water in reaction system are had studied2O and glacial acetic acid The mass ratio of the material is 1:10-200:5) and thermal crystallisation processing mode, at a lower temperature (70-150 DEG C), to 0.5at%Sn Adulterate TiO2The influence of the crystallinity of nano-powder, crystallite dimension and photocatalysis performance, gained TiO2Nano-powder can be applied to dirt The fields such as water process, air cleaning, antibacterial and deodouring, antifouling self-cleaning glass.
To achieve the goals above, present invention employs following technical solutions: a kind of Sn doping TiO2The system of nano-powder Preparation Method is prepared using the direct solution oxide method of high water, under stirring, by stannic chloride pentahydrate, water, glacial acetic acid and The pH that the mixed solution of butyl titanate is slowly dropped to 30 DEG C of constant temperature is to stir 1-4h in the acidic aqueous solution of 1.5-2.5, After still aging 24-100h, Sn doping TiO is obtained2Solution, then under 70-150 DEG C (such as: 75 DEG C, 150 DEG C) at thermal crystallisation 15h is managed, Sn doping TiO is obtained2Nano-powder, i.e. photocatalyst.
Wherein, the doping of the Sn is 0.5at%；The butyl titanate, H2The amount of the substance of O and glacial acetic acid Than for 1:(10-200): 5, such as 1:10:5,1:25:5,1:50:5,1:100:5,1:150:5,1:200:5；Five water The volume ratio for the acidic aqueous solution that tin tetrachloride, water, the mixed solution of glacial acetic acid and butyl titanate and pH are 1.5-2.5 is 3- 5:1.
Preferably, the pH of the acidic aqueous solution be 1.5-2.5, preferably 2.
Preferably, the acidic aqueous solution is the aqueous solution of glacial acetic acid.
Preferably, the revolving speed of the stirring is 100-600r/min.
Preferably, described to be slowly added dropwise to be added dropwise dropwise, such as 5-10mL/min.
Preferably, under stirring, by stannic chloride pentahydrate, H2O, the mixed solution of glacial acetic acid and butyl titanate is slow Slowly in the acidic aqueous solution that the pH for being added drop-wise to 30 DEG C of constant temperature is 2,2h, still aging 72h are stirred, obtains Sn doping TiO2Solution.
Preferably, the temperature of thermal crystallisation processing is 150 DEG C.
The invention further relates to the Sn of Sustainable use method as described above preparation to adulterate TiO2Nano-powder has crystallinity Height, the small feature of average grain diameter, average particle size range 2-7nm, preferably 5.91nm.
The invention further relates to protect Sn described above to adulterate TiO2Nano-powder is as photochemical catalyst in sewage treatment, sky Gas purification, antibacterial and deodouring are applied in antifouling self-cleaning glass, and wherein air cleaning includes degradation of formaldehyde, methyl orange.
Preferably, butyl titanate, H2O, the mass ratio of the material of glacial acetic acid is 1:150:5, and thermal crystallisation treatment temperature is 150 DEG C, TiO is adulterated by the Sn of the direct solution oxide method preparation of high water2Nano-powder, average grain diameter 5.91nm, photocatalysis Performance and crystallinity are best.
Preferably, Sn is adulterated into TiO2Nano-powder, water, dispersing agent (acrylic acid dispersant) are according to 10g:150- The ratio mixed grinding of 200mL:0.05-0.1mL, obtains slurry, is sprayed.The solution spraying is in ceramic tile, metope, glass, Metal, the surfaces such as wallpaper, nano particle can not have peeling phenomenon in close contact with surface after moisture drying.The photocatalyst solution is simultaneously Non-sterile water, therefore with being not suitable for being sprayed directly on to.Cooperate irradiating ultraviolet light effect more preferable, if therefore spraying indoors, answer It opens the window, solar radiation is allowed to come in.If the not interior of solar radiation or night, the irradiation of household mosquito killing lamp can be used, To reinforce ultraviolet light sources, general incandescent lamp also contains more low intensive ultraviolet light source, but necessary irradiation at short distance, photocatalyst Effect can be more preferable.Preferably, in order to improve the uniformity of spraying, polyethylene glycol PEG400 is added in spraying.According to volume ratio PEG400: slurry=2-20:100, optimal is 10:100.Photocatalyst and Fouling surfaces combine closer effect better, therefore spray After painting only have most surface particle could absorb decomposition of dirt, for guarantee photocatalysis effect, therefore spray when surface uniformity most To be important, much effect can be more preferable for the equalization spray of spray.
The present invention proposes a kind of to prepare nano-TiO2The new method of powder, beneficial effect are: the present invention is high for tradition TiO is prepared under warm (300 DEG C or more)2The defect of nano-powder, using the direct solution oxide method of high water, with butyl titanate and Stannic chloride pentahydrate is raw material (presoma), uses water to replace ethyl alcohol as solvent, glacial acetic acid is stabilizer, is made at 70-150 DEG C The 0.5at%Sn of standby different waters adulterates TiO2Sn is doped to TiO by nano-powder2In lattice, TiO is adjusted2Nano-powder is brilliant Particle size and crystallinity, so as to improve its photocatalysis performance.Pass through (70-150 DEG C) preparation better crystallinity degree of lower temperature and light The good TiO of catalytic performance2Nano-powder help to obtain small particle powder.The TiO of this method preparation2Photocatalyst average grain diameter model It encloses for 2-7nm, has good photocatalysis.Take 150 times of H at 150 DEG C2The Sn of O adulterates TiO2Nano-powder and undoped TiO2Nano-powder 10g, 200mL deionized water is ground 10min after 0.05mL dispersing agent (acrylic acid dispersant) mixing, is made Spray is sprayed on degradation of formaldehyde on wallpaper, the former works well.The Sn of this high direct solution oxide method preparation of water adulterates TiO2It receives Rice flour body has high catalytic activity, stable chemical performance, nontoxic, pollution-free, nonirritant, heat-resist, low in cost etc. excellent Point can be applied to the fields such as sewage treatment, air cleaning, antibacterial and deodouring, antifouling self-cleaning glass.
Detailed description of the invention
Fig. 1 is that the embodiment 1-6 different water Sns prepared in the case where 75 DEG C of thermal crystallisations are handled adulterate TiO2Nano-powder XRD spectrum；
Fig. 2 is that the embodiment 7-12 different water Sns prepared in the case where 150 DEG C of thermal crystallisations are handled adulterate TiO2Nano-powder XRD spectrum；
Fig. 3 is the pure TiO that comparative example does not have Sn to adulterate after 75 DEG C of thermal crystallisations are handled2The SEM of nano-powder schemes (a), and The 150 times of H after 75 DEG C of thermal crystallisations are handled of embodiment 52The TiO of O 0.5mol%Sn doping2The SEM of nano-powder schemes (b)；
Fig. 4 is the pure TiO that comparative example does not have Sn to adulterate after 75 DEG C of thermal crystallisations are handled2Nano-powder EDX map (a, And the 150 times of H after 75 DEG C of thermal crystallisations are handled of embodiment 5 b)2The TiO of O 0.5mol%Sn doping2Nano-powder EDX map (c, d)。
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description.
The present invention pass through first adjust butyl titanate, the ratio of water and glacial acetic acid obtain under different ratio (variable is Water and temperature) solution；Then to the TiO of different waters2Solution presoma carry out different temperatures heat treatment, then to heat at Manage obtained TiO2Nano-powder carries out XRD test, determines crystal structure, measures averagely according to thanking to Le formula D=K λ/β cos θ Crystallite dimension, wherein D is crystallite dimension (nm), and K is form factor constant, and taking 0.89, λ is X-ray wavelength, is taken 0.154056nm, β are the halfwidth (radian) of diffraction maximum, and θ is the angle of diffraction (degree) of X-ray, according to its crystallite dimension model of calculating It encloses for 2nm-7nm.
Embodiment 1
10 times of H at 75 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) 270mL deionized water is put into beaker, 15mL glacial acetic acid, which is added, makes solution ph be equal to 2, obtains acid water This beaker is placed on magnetic stirring apparatus and keeps stirring at 30 DEG C by solution, and the revolving speed of stirring is 300r/min.
(2) be put into 18mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and glacial acetic acid The mass ratio of the material (n) be 1:10:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by In the acidic aqueous solution that the step of being added drop-wise to stirring (1) obtains, after stirring 2h, still aging 72h, 0.5at% is obtained Sn adulterates TiO2Solution.
(4) 0.5at%Sn obtained in step (3) is adulterated into TiO2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 5.58nm.
Embodiment 2
25 times of H at 75 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 45mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and glacial acetic acid The mass ratio of the material (n) be 1:25:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5 at%Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 6.94nm.
Embodiment 3
50 times of H at 75 DEG C2O prepares 4at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 90mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and glacial acetic acid The mass ratio of the material (n) be 1:50:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by In the acidic aqueous solution that the step of being added drop-wise to stirring (1) obtains, after stirring 2h, still aging 72h, 0.5at% is obtained The TiO of Sn doping2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 5.20nm.
Embodiment 4
100 times of H at 75 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 180mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and glacial acetic acid The mass ratio of the material (n) be 1:100:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5 at%Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 4.52nm.
Embodiment 5
150 times of H at 75 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 270mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and ice vinegar The mass ratio of the material (n) of acid is 1:150:5)
(3) mixed solution of the stannic chloride pentahydrate, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) is dropwise It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains the TiO of 0.5at% Sn doping2 Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 4.80nm.
Embodiment 6
200 times of H at 75 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 360mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and glacial acetic acid The mass ratio of the material (n) be 1:200:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5at% Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 4.84nm.
Embodiment 7
10 times of H at 150 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) 270mL deionized water is put into beaker, 15mL glacial acetic acid, which is added, makes solution ph be equal to 2, obtains acid water This beaker is placed on magnetic stirring apparatus and keeps stirring at 30 DEG C by solution, and the revolving speed of stirring is 300r/min.
(2) be put into 18mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and glacial acetic acid The mass ratio of the material (n) be 1:10:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by In the acidic aqueous solution that the step of being added drop-wise to stirring (1) obtains, after stirring 2h, still aging 72h, 0.5at% is obtained The TiO of Sn doping2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 150 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 2.77nm.
Embodiment 8
25 times of H at 150 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 45mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and ice vinegar The mass ratio of the material (n) of acid is 1:25:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5 at%Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 150 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 3.18nm.
Embodiment 9
50 times of H at 150 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 90mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and ice vinegar The mass ratio of the material (n) of acid is 1:50:5)
(3) mixed solution of the stannic chloride pentahydrate, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) is dropwise In the acidic aqueous solution that the step of being added drop-wise to stirring (1) obtains, after stirring 2h, still aging 72h, 0.5at%Sn is obtained The TiO of doping2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 150 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 4.26nm.
Embodiment 10
100 times of H at 150 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 180mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and ice vinegar The mass ratio of the material (n) of acid is 1:100:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5 at%Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 150 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 5.34nm.
Embodiment 11
150 times of H at 150 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 270mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and ice vinegar The mass ratio of the material (n) of acid is 1:150:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5 at%Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 150 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 5.91nm.
Embodiment 12
200 times of H at 150 DEG C2O prepares 0.5at%Sn and adulterates TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acid equal to 2 Property aqueous solution, this beaker is placed on magnetic stirring apparatus and is kept stirring at 30 DEG C, the revolving speed of stirring is 300r/min.
(2) be put into 360mL deionized water in another beaker, be added stannic chloride pentahydrate solid 0.175g make it dissolve in In deionized water, 30mL glacial acetic acid is added later, first dissolution dissolution 15min adds butyl titanate 34mL, obtains five water four Stannic chloride, water, glacial acetic acid (HAc) and butyl titanate mixed solution.(wherein, butyl titanate, deionized water and ice vinegar The mass ratio of the material (n) of acid is 1:200:5)
(3) mixed solution of the stannic chloride pentahydrate, water, glacial acetic acid (HAc) and the butyl titanate that obtain step (2) by It is added drop-wise in the acidic aqueous solution that step (1) obtains, after stirring 2h, still aging 72h, obtains 0.5 at%Sn doping TiO2Solution.
(4) TiO for adulterating 0.5at%Sn obtained in step (3)2Solution handles 15h in 150 DEG C of thermal crystallisations, obtains 0.5at%Sn adulterates TiO2Nano-powder, average grain diameter 5.27nm.
Comparative example
150 times of H at 75 DEG C2O prepares pure TiO2The method of nano-powder, includes the following steps:
(1) it is put into 270mL deionized water in beaker, 15mL glacial acetic acid is added until solution ph obtains acidity equal to 2 This beaker is placed on magnetic stirring apparatus and keeps stirring at 30 DEG C by aqueous solution, and the revolving speed of stirring is 300r/min.
(2) it is put into 270mL deionized water in another beaker, 30mL glacial acetic acid is added, 34mL butyl titanate obtains The mixed solution of water, glacial acetic acid and butyl titanate.(wherein, the mass ratio of the material of butyl titanate, deionized water and glacial acetic acid It (n) is 1:150:5)
(3) mixed solution of water, glacial acetic acid and butyl titanate that step (2) obtains step (1) is added drop-wise to dropwise to obtain To acidic aqueous solution in, stir 2h, after still aging 72h, obtain pure TiO2Solution.
(4) by pure TiO obtained in step (3)2Solution handles 15h in 75 DEG C of thermal crystallisations, obtains pure TiO2Nano-powder, Average grain diameter is 5.2nm.
Embodiment 13
TiO is adulterated by 0.5at%Sn is prepared in embodiment 1-122Pulverizing for nano-powder, takes 0.5at% respectively Sn adulterates TiO2Powder 0.12g, 15mL deionized water is ground 72h after 0.05mL dispersing agent (acrylic acid dispersant) mixing, is obtained To slurry be respectively charged into blue mouth bottle, carry out photocatalysis experiment.Take 10mL slurry and 10mL concentration mixed for the methyl orange of 0.03g/L After conjunction, in the ultraviolet lighting 2h that 30W wavelength is 365nm, slurry is through 3000rms 8 minutes supernatants of centrifugation before and after measuring illumination respectively The absorbance of liquid calculates the degradation rate of methyl orange.Degradation rate=(A-B)/A, wherein A is the trap before illumination, and B is illumination Preceding trap.Be computed, the degradation rate of embodiment 1-12 is respectively as follows: 20.47%, 6.56%, 85.48%, 75.19%, 86.25%, 39.7%, 42.38%, 49.58%, 50%, 53.83%, 94.53%, 49.55%.
Embodiment 14
TiO is adulterated by 0.5at%Sn is prepared in embodiment 112Pulverizing for nano-powder, takes 0.5at%Sn to adulterate TiO2Powder 10g, 200mL deionized water grinds 10min after 0.05mL dispersing agent (acrylic acid dispersant) mixing, obtained slurry Material is respectively charged into watering can, is sprayed.The common common wallpaper in the market that spout alignment need to administer, the area of wallpaper is 1m2, Wallpaper double-faced uniform sprays 20mL slurry, and wallpaper is placed on 1m3Simple hand casing in, spray before survey glove box in formaldehyde concentration, For 0.29mg/m3, survey the concentration of the formaldehyde in glove box after spray again for 24 hours, be 0.09mg/m3。
Fig. 1 is the embodiment 1-6 different water Sns doping TiO prepared in 75 DEG C of thermal crystallisation processing2The XRD of nano-powder Map.By Fig. 1 reference standard card (PCPDF No.21-1272), H2O amount is respectively 10,25,50,100,150,200 times of Ti Molal quantity when, TiO2There is diffraction in 25.23 °, 38.91 °, 47.99 °, 55.15 °, 64.77 °, 75.05 ° in nano-powder Peak, the sample after doping also show as anatase crystal structure, and H2The TiO that O amount is 25,50,100,150,200 times2Nanometer Powder has good crystallinity, without SnO2Diffraction maximum occur, may be lauched in low temperature system and suitable Sn doping Divide evaporation slower, butyl titanate polycondensation reaction rate is slack-off, and Sn can preferably substitute Ti, makes the more thorough of tetrabutyl titanate hydrolysis Bottom, the time being transformed into from direct solution is elongated, and the nucleation of nanoparticle and growth are more preferable, and the Sn of preparation adulterates TiO2Nano powder Body has many advantages, such as that grain development is complete, and crystallinity is high.H2The TiO that O amount is 10 times2The diffraction maximum of nano-powder slightly moves to left, And crystallinity is poor, illustrates that butyl titanate generates nucleus TiO when water is very few2。H2O amount is respectively 10,25,50,100,150, When the molal quantity of 200 times of Ti, which is 20.47%, 6.56%, 85.48%, 75.19% to the degradation rate of methyl orange, 86.25%, 39.7%.
Fig. 2 is the embodiment 7-12 different water Sns doping TiO prepared in 150 DEG C of thermal crystallisation processing2Nano-powder XRD spectrum.By one reference standard card of figure (PCPDF No.21-1272), H2O amount is respectively 10,25,50,100,150,200 When the molal quantity of times Ti, TiO2Nano-powder spreads out in 25.23 °, 38.91 °, 47.99 °, 55.15 °, 64.77 °, 75.05 ° Peak is penetrated, diffraction maximum occurs, the sample after doping also shows as anatase crystal structure, and H2O amount is 50,100,150,200 TiO again2Nano-powder has good crystallinity, without SnO2Diffraction maximum occur, may be in low temperature system and suitable Sn Moisture evaporation is slower under doping, and polycondensation reaction rate is slack-off, and Sn can preferably substitute Ti, makes the more thorough of tetrabutyl titanate hydrolysis Bottom, the time being transformed into from direct solution is elongated, and the nucleation of nanoparticle and growth are more preferable, and the Sn of preparation adulterates TiO2Nano powder Body has many advantages, such as that grain development is complete, and crystallinity is high.H2O amount is the TiO of 10mol2The diffraction maximum of nano-powder slightly moves to left, And crystallinity is poor, when possible water is very few, butyl titanate is difficult to generate nucleus TiO2。H2O amount is respectively 10,25,50, When the molal quantity of 100,150,200 times of Ti, which is 42.38%, 49.58%, 50% to the degradation rate of methyl orange, 53.83%, 94.53%, 49.55%.
Fig. 3 (a) is it can be seen that the TiO that no Sn is adulterated2Nanoparticle agglomerates are obvious, and dispersion performance is bad, particle all compared with Greatly, crystallization degree is not high.Fig. 3 (b) is it can be seen that the Sn of preparation adulterates TiO2Nano particle is more loose, and particle size is smaller, Between 2-7nm, and crystal grain arbitrary orientation is grown, and crystallization degree is higher.
Fig. 4 is the pure TiO for not having Sn to adulterate after 75 DEG C of thermal crystallisations are handled2The EDX map (a, b) of nano-powder and 75 DEG C 150 times of H of 0.5mol%Sn after thermal crystallisation processing2The TiO of O2The EDX map (c, d) of nano-powder.It can be with from Fig. 4 (a) (b) Find out, the powder of preparation only has two kinds of elements of Ti and O, is evenly distributed, as can be seen that the powder of preparation has from Fig. 4 (c) (d) Tri- kinds of elements of Sn, Ti and O, are evenly distributed, illustrate that Sn has been doped into TiO2In crystal.
Pass through the direct solution oxide method preparation of high water, H2O amount and drying temperature have an impact to its structure and performance, same Under one drying temperature, with H2The increase of O amount, nano-powder structure are converted into anatase crystal, crystallization by unformed Degree and photo-catalysis capability are with H2The increase of O amount and enhance, in 150 times of H2Reach maximum under O amount.In 150 times of H2Under O amount, with The lower Sn prepared of 75 DEG C of dryings adulterates TiO2Nano-powder is compared, and the lower Sn prepared of 150 DEG C of dryings adulterates TiO2Nano-powder has Higher crystallinity and photocatalysis performance reach highest to the degradation rate of methyl orange, are 94.53% after ultraviolet lighting 2h.
The above only invents preferable specific embodiment, basic principle, the spy of main feature and degradation of formaldehyde Point.But scope of protection of the present invention is not limited thereto, anyone skilled in the art the invention discloses In technical scope, it is subject to equivalent substitution or change according to the technical scheme of the invention and its inventive conception, should all covers in this hair Within bright protection scope.

Claims (8)

1. a kind of Sn adulterates TiO2The preparation method of nano-powder, which is characterized in that under stirring, by stannic chloride pentahydrate, The mixed solution of water, glacial acetic acid and butyl titanate be slowly dropped to 30 DEG C of constant temperature pH be 1.5-2.5 acidic aqueous solution in, 1-4h is stirred, after standing 24-100h, obtains Sn doping TiO2Solution, then thermal crystallisation handles 15h at 70-150 DEG C, obtains Sn Adulterate TiO2Nano-powder；
Wherein, the doping of the Sn is 0.5at%；The mass ratio of the material of the butyl titanate, water and glacial acetic acid is 1: 10-200:5；The volume ratio of the stannic chloride pentahydrate, water, the mixed solution of glacial acetic acid and butyl titanate and acidic aqueous solution For 3-5:1.
2. Sn according to claim 1 adulterates TiO2The preparation method of nano-powder, which is characterized in that the acid water Solution is the aqueous solution of glacial acetic acid.
3. Sn according to claim 1 adulterates TiO2The preparation method of nano-powder, which is characterized in that the slow drop It adds as being added dropwise dropwise.
4. Sn according to claim 1 adulterates TiO2The preparation method of nano-powder, which is characterized in that the stirring Revolving speed is 100-600r/min.
5. the Sn of the preparation of method described in any one of claim 1-4 adulterates TiO2Nano-powder.
6. Sn according to claim 5 adulterates TiO2Nano-powder, which is characterized in that the Sn adulterates TiO2Nano powder The average grain diameter of body is 2-7nm.
7. Sn described in claim 5 or 6 adulterates TiO2Nano-powder is as photochemical catalyst in sewage treatment, air cleaning, antibacterial It is applied in deodorization, antifouling self-cleaning glass.
8. Sn as claimed in claim 7 adulterates TiO2Nano-powder is applied in degradation of formaldehyde, methyl orange as photochemical catalyst.
CN201910669234.8A 2019-07-24 2019-07-24 The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application Pending CN110314676A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910669234.8A CN110314676A (en) 2019-07-24 2019-07-24 The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910669234.8A CN110314676A (en) 2019-07-24 2019-07-24 The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application

Publications (1)

Publication Number Publication Date
CN110314676A true CN110314676A (en) 2019-10-11

Family

ID=68124306

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910669234.8A Pending CN110314676A (en) 2019-07-24 2019-07-24 The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application

Country Status (1)

Country Link
CN (1) CN110314676A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115057471A (en) * 2022-05-23 2022-09-16 山东大学 Lithium ion battery cathode material and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101062476A (en) * 2007-05-15 2007-10-31 河北大学 Metallic ion doped nano TiO2 transparent photo-catalytic emulsion and preparation method thereof
CN101108336A (en) * 2007-07-11 2008-01-23 南开大学 Method of manufacturing nitrogen of high activity, stannum ion codope nano titanium dioxide photocatalyst
JP2013126654A (en) * 2011-11-14 2013-06-27 Shin-Etsu Chemical Co Ltd Visible-light-responsive titanium oxide microparticle dispersion, method for manufacturing same, and member having surficial photocatalyst thin film formed using same dispersion
CN103394343A (en) * 2013-08-16 2013-11-20 河海大学 Preparation method and application of metal-doped titanium dioxide material
CN103691419A (en) * 2013-11-30 2014-04-02 常熟市华宇针织印染有限公司 Preparation method of visible light degrading agent for printing and dyeing wastewater treatment
CN103806270A (en) * 2014-02-18 2014-05-21 南通纺织职业技术学院 Modified titanium dioxide hydrosol and preparation method thereof
CN106076311A (en) * 2016-06-29 2016-11-09 渤海大学 A kind of preparation method of titanium dioxide/tin ash complex oxide ultrafine nano-particle

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101062476A (en) * 2007-05-15 2007-10-31 河北大学 Metallic ion doped nano TiO2 transparent photo-catalytic emulsion and preparation method thereof
CN101108336A (en) * 2007-07-11 2008-01-23 南开大学 Method of manufacturing nitrogen of high activity, stannum ion codope nano titanium dioxide photocatalyst
JP2013126654A (en) * 2011-11-14 2013-06-27 Shin-Etsu Chemical Co Ltd Visible-light-responsive titanium oxide microparticle dispersion, method for manufacturing same, and member having surficial photocatalyst thin film formed using same dispersion
CN103394343A (en) * 2013-08-16 2013-11-20 河海大学 Preparation method and application of metal-doped titanium dioxide material
CN103691419A (en) * 2013-11-30 2014-04-02 常熟市华宇针织印染有限公司 Preparation method of visible light degrading agent for printing and dyeing wastewater treatment
CN103806270A (en) * 2014-02-18 2014-05-21 南通纺织职业技术学院 Modified titanium dioxide hydrosol and preparation method thereof
CN106076311A (en) * 2016-06-29 2016-11-09 渤海大学 A kind of preparation method of titanium dioxide/tin ash complex oxide ultrafine nano-particle

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
NADIR KIRAZ ET AL.: "Preparation of Sn doped nanometric TiO2 powders by reflux and hydrothermal syntheses and their characterization", 《J SOL-GEL SCI TECHNOL》 *
吴宏富等: "《中国粉体工业通鉴 第二卷（2006版）》", 30 June 2006, 中国建材工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115057471A (en) * 2022-05-23 2022-09-16 山东大学 Lithium ion battery cathode material and preparation method thereof

Similar Documents

Publication Publication Date Title
JP4803180B2 (en) Titanium oxide photocatalyst, its production method and use
RU2431604C2 (en) METHOD OF PREPARING AQUEOUS DISPERSIONS OF TiO2 IN FORM OF NANOPARTICLES AND DISPERSIONS OBTAINED USING SAID METHOD
Xie et al. Facile process to greatly improve the photocatalytic activity of the TiO2 thin film on window glass for the photodegradation of acetone and benzene
NO333658B1 (en) Mixture for coating walls, method of preparation and use of the same
US20120168666A1 (en) Coating composition and uses thereof
JPWO2005102521A1 (en) Titanium oxide photocatalyst, method for producing the same, and use thereof
Ge et al. Fabrication and characterization of nano TiO2 thin films at low temperature
Mufti et al. The effect of TiO2 thin film thickness on self-cleaning glass properties
CN109174075A (en) A kind of rare-earth element modified titanium dioxide nano photocatalysis material and preparation method thereof for photocatalytic degradation VOCs
CN104071836A (en) Titanium dioxide hollow nanosphere and preparation method thereof
Chaudhari et al. Effect of annealing on the photocatalytic activity of chemically prepared TiO2 thin films under visible light
CN106311100B (en) A kind of production method of photocatalysis complex microsphere
Ge et al. Low-temperature synthesis of photocatalytic TiO 2 thin film from aqueous anatase precursor sols
CN105289457B (en) A kind of hollow structure TiO2The preparation method and applications of nano material
Rise et al. Synthesis and characterization of ZnO nanorods-Zn2SiO4 nanoparticles-PMMA nanocomposites for UV-C protection
CA2735747A1 (en) Titanium dioxide coatings and methods of forming titanium dioxide coatings having reduced crystallite size
TWI291895B (en) Sol containing titanium oxide, thin film formed therefrom and production process of the sol
CN110314677B (en) TiO2 nano powder with different Sn doping amounts prepared by direct solution oxidation method and application thereof
CN110314676A (en) The high direct solution oxide method preparation Sn of water adulterates TiO2Nano-powder and its application
WO2009017458A1 (en) Solution of particles containing titanium dioxide and peroxo-titanium complex, and its preparation
CN105271400A (en) Preparation method of mixed crystal nano-TiO2
CN105399138A (en) Perovskite SrTiO3 tetragonal nanoparticle preparation method and product
JP2007268523A (en) Photocatalyst dispersion
KR20190061691A (en) sol composition of photo-catalystic material, method of preparing the same, and Method of preparing thin layer of Photo-catalyst using the same
Kao et al. Characterization, photoelectrochemical properties, and surface wettabilities of transparent porous TiO2 thin films

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: 20191011

WD01 Invention patent application deemed withdrawn after publication