CN111392772A - Preparation method of nano titanium dioxide material with uniform particle size distribution - Google Patents
Preparation method of nano titanium dioxide material with uniform particle size distribution Download PDFInfo
- Publication number
- CN111392772A CN111392772A CN202010263065.0A CN202010263065A CN111392772A CN 111392772 A CN111392772 A CN 111392772A CN 202010263065 A CN202010263065 A CN 202010263065A CN 111392772 A CN111392772 A CN 111392772A
- Authority
- CN
- China
- Prior art keywords
- temperature
- foaming body
- titanium dioxide
- particle size
- size distribution
- 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.)
- Withdrawn
Links
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 title claims abstract description 35
- 238000009826 distribution Methods 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 115
- 238000005187 foaming Methods 0.000 claims abstract description 56
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 49
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 49
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 235000019441 ethanol Nutrition 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 21
- PSLIMVZEAPALCD-UHFFFAOYSA-N ethanol;ethoxyethane Chemical compound CCO.CCOCC PSLIMVZEAPALCD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000005507 spraying Methods 0.000 claims abstract description 13
- 238000007664 blowing Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000006260 foam Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000011010 flushing procedure Methods 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 16
- 239000004408 titanium dioxide Substances 0.000 description 10
- 238000011065 in-situ storage Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
- B01J35/394—Metal dispersion value, e.g. percentage or fraction
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a nano titanium dioxide material with uniform particle size distribution, which comprises the following steps: adding polyvinylpyrrolidone into anhydrous ethanol, and performing low-temperature ultrasonic dispersion for 10-20min to obtain polyvinylpyrrolidone ethanol dispersion liquid; soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 20-30min, taking out, and quickly drying to obtain a coated porous foaming body; adding n-butyl titanate into the ethanol-ether mixed solution, and uniformly stirring at a low temperature to form a titanium solution; uniformly spraying titanium liquid on the surface of the coated porous foam body to form a surface liquid film, and drying to obtain a n-butyl titanate film; adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 30-60min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body; soaking the double-membrane foaming body into absolute ethyl alcohol, stirring at constant temperature for 30-60min, taking out the foaming body, filtering to obtain a precipitate, washing with absolute ethyl alcohol, and drying to obtain the nano titanium dioxide with uniform particle size distribution.
Description
Technical Field
The invention belongs to a nano material, relates to the field of photocatalysis, and particularly relates to a preparation method of a nano titanium dioxide material with uniform particle size distribution.
Background
TiO as one of semiconductor photocatalysts2The photocatalytic material is a novel environment-friendly material which is most researched at present, and the property of the photocatalyst is a key factor in the photocatalytic oxidation process. TiO 22The crystal form, the grain size, the grain diameter, the surface state and other factors have great influence on the photocatalytic performance. The nano-particle with large surface area has good catalytic activity and selectivity due to the surface effect and the volume effect. Nano TiO 22The energy levels of the conduction band and the valence band of the crystal become separated due to the quantum size effectThe vertical energy level, the energy gap is widened, the conducting band potential becomes more negative, and the valence band potential becomes more positive, which means that the material has stronger oxidation and reduction capability; and because the particle size of the nano particles is small, a photon-generated carrier is easier to migrate to the surface from the inside of the particles than coarse particles, the recombination probability of electrons and holes is obviously reduced, and the photocatalysis performance is also improved. Thus, TiO having a large specific surface area and a small particle diameter is produced2Has been the focus of research in the field of photocatalysis.
The current titanium dioxide preparation methods comprise the traditional solid phase reaction and sintering method and the modern chemical vapor deposition method, physical vapor deposition method, chemical vapor infiltration method, sol-gel method and the like. These methods are extremely complicated in process and uneven in particle size distribution, resulting in large differences in the specific surface area of titanium dioxide.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a nano titanium dioxide material with uniform particle size distribution, which solves the problem of non-uniform particle size distribution of titanium dioxide, forms in-situ nano titanium dioxide by utilizing in-situ hydrolysis of a tetrabutyl titanate liquid film, and effectively prevents agglomeration of the nano titanium dioxide based on in-situ curing effect.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a method for preparing a nano titanium dioxide material with uniform particle size distribution comprises the following steps:
step 1, adding polyvinylpyrrolidone into absolute ethyl alcohol, and performing low-temperature ultrasonic dispersion for 10-20min to obtain polyvinylpyrrolidone ethanol dispersion liquid, wherein the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 10-20 g/L, the ultrasonic frequency of ultrasonic dispersion is 50-80kHz, and the temperature is 40-60 ℃;
step 2, soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 20-30min, taking out, and quickly drying to obtain a coated porous foaming body; standing at 20-30 deg.C, and rapidly drying at 80-100 deg.C;
step 3, adding n-butyl titanate into the ethanol-diethyl ether mixed solution, and uniformly stirring at a low temperature to form a titanium solution, wherein the concentration of the n-butyl titanate in the ethanol-diethyl ether mixed solution is 20-30 g/L, the volume ratio of ethanol in the ethanol-diethyl ether mixed solution is 5-10%, the low-temperature stirring temperature is 10-20 ℃, and the stirring speed is 1000-2000 r/min;
step 4, uniformly spraying titanium liquid on the surface of the coated porous foaming body to form a surface liquid film, and drying to obtain the n-butyl titanate film, wherein the spraying amount of the titanium liquid is 15-25m L/cm2The drying temperature is 100-120 ℃;
step 5, adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 30-60min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body; the humidity of the humid air is 20-30%, the temperature is 60-70 ℃, and the temperature of the constant-temperature nitrogen is 100-120 ℃;
step 6, soaking the double-membrane foaming body into absolute ethyl alcohol, stirring at constant temperature for 30-60min, taking out the foaming body, filtering to obtain a precipitate, washing with absolute ethyl alcohol, and drying to obtain nano titanium dioxide with uniform particle size distribution; the constant-temperature stirring temperature is 30-50 ℃, and the drying temperature is 100-120 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of uneven distribution of the particle size of titanium dioxide, forms in-situ nano titanium dioxide by utilizing in-situ hydrolysis of a tetrabutyl titanate liquid film, and effectively prevents the agglomeration of the nano titanium dioxide based on in-situ curing effect.
2. The invention utilizes polyvinylpyrrolidone as an adhesive and a dispersant, effectively improves the dispersion of the nano titanium dioxide in the absolute ethyl alcohol, can recycle the polyvinylpyrrolidone and greatly reduces the cost.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
A method for preparing a nano titanium dioxide material with uniform particle size distribution comprises the following steps:
step 1, adding polyvinylpyrrolidone into absolute ethyl alcohol, and performing low-temperature ultrasonic dispersion for 10-20min to obtain polyvinylpyrrolidone ethanol dispersion liquid, wherein the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 10-20 g/L, the ultrasonic frequency of ultrasonic dispersion is 50-80kHz, the temperature is 40-60 ℃, polyvinylpyrrolidone has good solubility in absolute ethyl alcohol, ultrasonic dispersion can generate clutch energy, and polyvinylpyrrolidone is rapidly dispersed into absolute ethyl alcohol through the clutch energy to achieve the purpose of uniform dispersion;
step 2, soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 20-30min, taking out, and quickly drying to obtain a coated porous foaming body; standing at 20-30 deg.C, rapidly drying at 80-100 deg.C, soaking the porous foam in ethanol solution of polyvinylpyrrolidone to form a liquid film on the surface of the porous foam by the film forming property of ethanol, wherein the liquid film contains polyvinylpyrrolidone, and rapidly drying to form polyvinylpyrrolidone film on the surface of the porous foam;
step 3, adding n-butyl titanate into the ethanol-diethyl ether mixed solution, and uniformly stirring at low temperature to form a titanium liquid, wherein the concentration of the n-butyl titanate in the ethanol-diethyl ether mixed solution is 20-30 g/L, the volume ratio of ethanol in the ethanol-diethyl ether mixed solution is 5-10%, the stirring temperature at low temperature is 10-20 ℃, and the stirring speed is 2000r/min, the n-butyl titanate has good solubility in ethanol and diethyl ether, can be converted into a solution, and can be uniformly dispersed into the whole solution in a low-temperature stirring manner to form a uniform solution, meanwhile, the ethanol and the diethyl ether can achieve the effect of mutual dissolution, so that the whole solution can not be layered, and the solution is ensured to be uniform;
step 4, uniformly spraying titanium liquid on the surface of the coated porous foaming body to form a surface liquid film, and drying to obtain an n-butyl titanate film, wherein the spraying amount of the titanium liquid is 15-25m L/cm 2, the drying temperature is 100-120 ℃, the titanium liquid is uniformly sprayed on the coated porous foaming body to form a liquid film on the surface of the porous foaming body, meanwhile, the surface expansion can be formed on polyvinylpyrrolidone based on the solubility of ethanol to polyvinylpyrrolidone, gaps among polyvinylpyrrolidone molecules are opened, n-butyl titanate permeates into the gaps, meanwhile, the n-butyl titanate can be flatly spread on the surface of the polyvinylpyrrolidone due to the insolubility of the diethyl ether and the polyvinylpyrrolidone to form a surface n-butyl titanate ethyl ether film, the diethyl ether and the ethanol are gradually evaporated in the drying process to form the n-butyl titanate film with a part interlaced with the polyvinylpyrrolidone, and ethyl ether and ethanol steam in the drying process are condensed and then are reused for preparing an ethanol-diethyl ether mixed solution;
step 5, adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 30-60min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body; the humidity of the humid air is 20-30%, the temperature is 60-70 ℃, and the temperature of the constant-temperature nitrogen is 100-120 ℃; the wet air contains water vapor, the tetrabutyl titanate is hydrolyzed when meeting water molecules in the standing process to form titanic acid, and is converted into nano titanium dioxide in the nitrogen tail blowing process, and meanwhile, the polyvinylpyrrolidone has certain solubility in water, so that in the wet air, the water molecules are adsorbed on the polyvinylpyrrolidone and permeate into the polyvinylpyrrolidone molecules to hydrolyze the tetrabutyl titanate in gaps of the polyvinylpyrrolidone; therefore, after constant-temperature nitrogen tail blowing, a polyvinylpyrrolidone film and a nano titanium dioxide film are formed on the surface of the foaming body;
step 6, soaking the double-membrane foaming body into absolute ethyl alcohol, stirring at constant temperature for 30-60min, taking out the foaming body, filtering to obtain a precipitate, washing with absolute ethyl alcohol, and drying to obtain nano titanium dioxide with uniform particle size distribution; the constant-temperature stirring temperature is 30-50 ℃, and the drying temperature is 100-120 ℃; the double-film foaming body is soaked in absolute ethyl alcohol, in the process, polyvinylpyrrolidone is dissolved in the absolute ethyl alcohol, so that the nano titanium dioxide can be separated from the foaming body, the dispersing effect of the nano titanium dioxide in the absolute ethyl alcohol is achieved, and meanwhile, the polyvinylpyrrolidone has dispersibility, so that the uniform dispersion of the nano titanium dioxide can be improved; filtering to obtain nanometer titanium dioxide precipitate, washing and drying to obtain nanometer titanium dioxide material with uniform particle size distribution.
Example 1
A method for preparing a nano titanium dioxide material with uniform particle size distribution comprises the following steps:
step 1, adding polyvinylpyrrolidone into 1L absolute ethyl alcohol, and performing low-temperature ultrasonic dispersion for 10min to obtain polyvinylpyrrolidone ethanol dispersion liquid, wherein the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 10 g/L, the ultrasonic frequency of ultrasonic dispersion is 50kHz, and the temperature is 40 ℃;
step 2, soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 20min, taking out, and quickly drying to obtain a coated porous foaming body; standing at 20 deg.C, and rapidly drying at 80 deg.C;
step 3, adding n-butyl titanate into the ethanol-diethyl ether mixed solution, and uniformly stirring at a low temperature to form a titanium solution, wherein the concentration of the n-butyl titanate in the ethanol-diethyl ether mixed solution is 20 g/L, the volume ratio of ethanol in the ethanol-diethyl ether mixed solution is 5%, the low-temperature stirring temperature is 10 ℃, and the stirring speed is 1000 r/min;
step 4, uniformly spraying titanium liquid on the surface of the coated porous foam body to form a surface liquid film, and drying to obtain the n-butyl titanate film, wherein the spraying amount of the titanium liquid is 15m L/cm2The drying temperature is 100 ℃;
step 5, adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 30min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body; the humidity of the humid air is 20%, the temperature is 60 ℃, and the temperature of constant-temperature nitrogen is 100 ℃;
step 6, soaking the double-membrane foaming body into absolute ethyl alcohol, stirring for 30min at constant temperature, taking out the foaming body, filtering to obtain a precipitate, washing with absolute ethyl alcohol, and drying to obtain nano titanium dioxide with uniform particle size distribution; the constant-temperature stirring temperature is 30 ℃, and the drying temperature is 100 ℃.
The titanium dioxide of this example has a particle size of 100-200nm and a distribution of 95%.
Example 2
A method for preparing a nano titanium dioxide material with uniform particle size distribution comprises the following steps:
step 1, adding polyvinylpyrrolidone into absolute ethyl alcohol, and performing low-temperature ultrasonic dispersion for 20min to obtain polyvinylpyrrolidone ethanol dispersion liquid, wherein the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 20 g/L, the ultrasonic frequency of ultrasonic dispersion is 80kHz, and the temperature is 60 ℃;
step 2, soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 30min, taking out, and quickly drying to obtain a coated porous foaming body; standing at 30 deg.C, and rapidly drying at 100 deg.C;
step 3, adding n-butyl titanate into the ethanol-diethyl ether mixed solution, and uniformly stirring at a low temperature to form a titanium solution, wherein the concentration of the n-butyl titanate in the ethanol-diethyl ether mixed solution is 30 g/L, the volume ratio of ethanol in the ethanol-diethyl ether mixed solution is 10%, the low-temperature stirring temperature is 20 ℃, and the stirring speed is 2000 r/min;
step 4, uniformly spraying titanium liquid on the surface of the coated porous foam body to form a surface liquid film, and drying to obtain the n-butyl titanate film, wherein the spraying amount of the titanium liquid is 25m L/cm2The drying temperature is 120 ℃;
step 5, adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 60min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body; the humidity of the humid air is 30%, the temperature is 70 ℃, and the temperature of constant-temperature nitrogen is 120 ℃;
step 6, soaking the double-membrane foaming body into absolute ethyl alcohol, stirring at constant temperature for 60min, taking out the foaming body, filtering to obtain a precipitate, washing with absolute ethyl alcohol, and drying to obtain nano titanium dioxide with uniform particle size distribution; the constant-temperature stirring temperature is 50 ℃, and the drying temperature is 120 ℃.
The titanium dioxide of the present example has a particle size range of 300-500nm and a distribution rate of 96%.
Example 3
A method for preparing a nano titanium dioxide material with uniform particle size distribution comprises the following steps:
step 1, adding polyvinylpyrrolidone into absolute ethyl alcohol, and performing low-temperature ultrasonic dispersion for 15min to obtain polyvinylpyrrolidone ethanol dispersion liquid, wherein the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 15 g/L, the ultrasonic frequency of ultrasonic dispersion is 70kHz, and the temperature is 50 ℃;
step 2, soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 25min, taking out, and quickly drying to obtain a coated porous foaming body; standing at 25 deg.C, and rapidly drying at 90 deg.C;
step 3, adding n-butyl titanate into the ethanol-diethyl ether mixed solution, and uniformly stirring at a low temperature to form a titanium solution, wherein the concentration of the n-butyl titanate in the ethanol-diethyl ether mixed solution is 24 g/L, the volume ratio of ethanol in the ethanol-diethyl ether mixed solution is 8%, the low-temperature stirring temperature is 15 ℃, and the stirring speed is 1500 r/min;
step 4, uniformly spraying titanium liquid on the surface of the coated porous foam body to form a surface liquid film, and drying to obtain the n-butyl titanate film, wherein the spraying amount of the titanium liquid is 20m L/cm2The drying temperature is 110 ℃;
step 5, adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 50min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body; the humidity of the humid air is 25%, the temperature is 65 ℃, and the temperature of constant-temperature nitrogen is 110 ℃;
step 6, soaking the double-membrane foaming body into absolute ethyl alcohol, stirring for 40min at constant temperature, taking out the foaming body, filtering to obtain a precipitate, washing with absolute ethyl alcohol, and drying to obtain nano titanium dioxide with uniform particle size distribution; the constant-temperature stirring temperature is 40 ℃, and the drying temperature is 110 ℃.
The titanium dioxide of this example has a particle size of 150-300nm and a distribution of 95%.
In summary, the invention has the following advantages:
1. the invention solves the problem of uneven distribution of the particle size of titanium dioxide, forms in-situ nano titanium dioxide by utilizing in-situ hydrolysis of a tetrabutyl titanate liquid film, and effectively prevents the agglomeration of the nano titanium dioxide based on in-situ curing effect.
2. The invention utilizes polyvinylpyrrolidone as an adhesive and a dispersant, effectively improves the dispersion of the nano titanium dioxide in the absolute ethyl alcohol, can recycle the polyvinylpyrrolidone and greatly reduces the cost.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (7)
1. A method for preparing a nano titanium dioxide material with uniform particle size distribution is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding polyvinylpyrrolidone into absolute ethyl alcohol, and performing low-temperature ultrasonic dispersion for 10-20min to obtain polyvinylpyrrolidone ethanol dispersion liquid;
step 2, soaking the porous foaming body into polyvinylpyrrolidone ethanol dispersion liquid, standing for 20-30min, taking out, and quickly drying to obtain a coated porous foaming body;
step 3, adding n-butyl titanate into the ethanol-ether mixed solution, and uniformly stirring at a low temperature to form a titanium solution;
step 4, uniformly spraying titanium liquid on the surface of the coated porous foam body to form a surface liquid film, and drying to obtain the n-butyl titanate film;
step 5, adding the foaming body with the n-butyl titanate film into a reaction kettle, flushing damp air, standing the foaming body for 30-60min, and blowing tail by constant-temperature nitrogen to obtain a double-film foaming body;
and 6, soaking the double-membrane foaming body into absolute ethyl alcohol, stirring at constant temperature for 30-60min, taking out the foaming body, filtering to obtain a precipitate, washing with the absolute ethyl alcohol, and drying to obtain the nano titanium dioxide with uniform particle size distribution.
2. The method for preparing the nano titanium dioxide material with uniform particle size distribution according to claim 1, wherein the concentration of the polyvinylpyrrolidone in the absolute ethyl alcohol in the step 1 is 10-20 g/L, the ultrasonic frequency of the ultrasonic dispersion is 50-80kHz, and the temperature is 40-60 ℃.
3. The method for preparing nano titanium dioxide material with uniform particle size distribution according to claim 1, wherein the method comprises the following steps: the temperature of standing in the step 2 is 20-30 ℃, and the temperature of quick drying is 80-100 ℃.
4. The method for preparing nano titanium dioxide material with uniform particle size distribution as claimed in claim 1, wherein the concentration of n-butyl titanate in the ethanol-ether mixture in step 3 is 20-30 g/L, the volume ratio of ethanol in the ethanol-ether mixture is 5-10%, the low-temperature stirring temperature is 10-20 ℃, and the stirring speed is 1000-2000 r/min.
5. The method for preparing nano titanium dioxide material with uniform particle size distribution according to claim 1, wherein the spraying amount of the titanium solution in the step 4 is 15-25m L/cm2The drying temperature is 100-120 ℃.
6. The method for preparing nano titanium dioxide material with uniform particle size distribution according to claim 1, wherein the method comprises the following steps: the humidity of the humid air in the step 5 is 20-30%, the temperature is 60-70 ℃, and the temperature of the constant-temperature nitrogen is 100-120 ℃.
7. The method for preparing nano titanium dioxide material with uniform particle size distribution according to claim 1, wherein the method comprises the following steps: the temperature of the constant-temperature stirring in the step 6 is 30-50 ℃, and the drying temperature is 100-120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010263065.0A CN111392772A (en) | 2020-04-07 | 2020-04-07 | Preparation method of nano titanium dioxide material with uniform particle size distribution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010263065.0A CN111392772A (en) | 2020-04-07 | 2020-04-07 | Preparation method of nano titanium dioxide material with uniform particle size distribution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111392772A true CN111392772A (en) | 2020-07-10 |
Family
ID=71425161
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010263065.0A Withdrawn CN111392772A (en) | 2020-04-07 | 2020-04-07 | Preparation method of nano titanium dioxide material with uniform particle size distribution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111392772A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250101A (en) * | 2020-10-29 | 2021-01-22 | 焦祝根 | Method for in-situ preparation of nano zinc chloride |
| CN114956155A (en) * | 2022-06-21 | 2022-08-30 | 中国船舶重工集团公司第七二五研究所 | Composite anti-fouling agent and preparation method thereof |
| CN117772172A (en) * | 2024-02-23 | 2024-03-29 | 山西安仑化工有限公司 | Preparation method and preparation device of titanium oxide/magnetic carbon black catalytic material |
-
2020
- 2020-04-07 CN CN202010263065.0A patent/CN111392772A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250101A (en) * | 2020-10-29 | 2021-01-22 | 焦祝根 | Method for in-situ preparation of nano zinc chloride |
| CN114956155A (en) * | 2022-06-21 | 2022-08-30 | 中国船舶重工集团公司第七二五研究所 | Composite anti-fouling agent and preparation method thereof |
| CN117772172A (en) * | 2024-02-23 | 2024-03-29 | 山西安仑化工有限公司 | Preparation method and preparation device of titanium oxide/magnetic carbon black catalytic material |
| CN117772172B (en) * | 2024-02-23 | 2024-05-03 | 山西安仑化工有限公司 | Preparation method and preparation device of titanium oxide/magnetic carbon black catalytic material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111392772A (en) | Preparation method of nano titanium dioxide material with uniform particle size distribution | |
| CN106976907B (en) | A kind of nano-titanium dioxide preparation method of size tunable | |
| CN105833918B (en) | A kind of compounded visible light photocatalyst Ag2CO3/TiO2/ UiO-66-(COOH)2Preparation method and applications | |
| CN108514887B (en) | Hollow nanoparticle titanium dioxide/black phosphorus alkene photo-thermal catalyst and preparation method and application thereof | |
| CN108502923B (en) | Preparation method of nano titanium dioxide material with uniform particle size distribution | |
| CN111054417B (en) | High-efficiency iron monatomic Fenton catalyst, and synthesis method and application thereof | |
| CN103861630A (en) | Copolymerization-modified graphite-phase carbon nitride hollow ball visible light-driven photocatalyst | |
| CN108483490A (en) | A kind of preparation method of nano-titanium dioxide | |
| CN109201029B (en) | Preparation method of efficient porous composite photocatalytic material | |
| CN109179495B (en) | Preparation method of high-dispersion nano titanium dioxide | |
| CN103801354B (en) | A kind of graphite phase carbon nitride hollow ball visible light catalyst of after annealing process | |
| CN108609650B (en) | Preparation method of nano titanium dioxide | |
| CN107180916A (en) | A kind of flexible infiltration perovskite photovoltaic material | |
| CN108579738B (en) | Gold nanoparticle/titanium dioxide nanoflower composite material and preparation method and application thereof | |
| CN105879918B (en) | A kind of compounded visible light photocatalyst Ag2CO3/TiO2/ UIO-66-(COOH)2And organic matter degradation application | |
| CN108404948B (en) | One kind (BiO)2CO3-BiO2-xComposite photocatalyst and preparation method and application thereof | |
| CN110871099A (en) | Ag-containing material3PO4And carboxylated g-C3N4Preparation method of photocatalytic degradation nano-fiber | |
| CN108103766B (en) | Molybdenum disulfide composite fiber photocatalyst for sewage treatment and preparation method thereof | |
| CN112742364B (en) | Preparation method of novel mesoporous photocatalyst carrier | |
| CN108408749A (en) | A kind of preparation method of superfine alumina powder | |
| CN112940296B (en) | Preparation method of nano polylactic acid | |
| CN114522666A (en) | Preparation method of multistage porous carbon fiber cloth integrating adsorption and degradation of formaldehyde | |
| CN113856732A (en) | Lamellar flower-shaped Mn (VO)3)2Composite g-C3N4Photocatalyst and preparation method and application thereof | |
| CN115155644B (en) | Improve g-C 3 N 4 Method for catalytic activation of photocatalytic fiber membrane | |
| CN105819564A (en) | Treatment method for paraformaldehyde wastewater |
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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200710 |
|
| WW01 | Invention patent application withdrawn after publication |