WO2022007761A1 - Méthode et dispositif de préparation de dioxyde de titane nanométrique monodispersé - Google Patents
Méthode et dispositif de préparation de dioxyde de titane nanométrique monodispersé Download PDFInfo
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- WO2022007761A1 WO2022007761A1 PCT/CN2021/104591 CN2021104591W WO2022007761A1 WO 2022007761 A1 WO2022007761 A1 WO 2022007761A1 CN 2021104591 W CN2021104591 W CN 2021104591W WO 2022007761 A1 WO2022007761 A1 WO 2022007761A1
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- titanium dioxide
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- hydrochloric acid
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 99
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000463 material Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 27
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims description 34
- 239000004408 titanium dioxide Substances 0.000 claims description 28
- -1 titanium oxide compound Chemical class 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 20
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 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 claims description 4
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 3
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical class Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 230000007774 longterm Effects 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 230000002269 spontaneous effect Effects 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 42
- 239000000047 product Substances 0.000 description 36
- 239000012071 phase Substances 0.000 description 26
- 239000002105 nanoparticle Substances 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 12
- 238000002834 transmittance Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000001246 colloidal dispersion Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000013517 stratification Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003916 acid precipitation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- 239000000516 sunscreening agent Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Images
Classifications
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- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
Definitions
- the invention relates to a preparation method and device of monodisperse nano titanium dioxide.
- Nano titanium dioxide has special effects such as small particle size, high specific surface area, excellent photocatalytic activity, stable chemical and thermal properties, super affinity, etc. irreplaceable application advantages.
- nano-titanium dioxide can be used to decompose formaldehyde, benzene, TVOC, SOx, NOx, etc.
- nano-titanium dioxide is used in glass, shutters, Mirrors, street lamps and other surfaces can achieve self-cleaning effect; nano-titanium dioxide is also widely used in medical equipment, catheters, operating rooms, sunscreen cosmetics, sunscreen clothing, whitening products, anti-aging coatings and other fields; in addition, nano-titanium dioxide can also be used in lithium Energy conversion and storage fields such as anode materials for ion batteries, photocatalysis or photoelectric catalytic production of hydrogen energy.
- the preparation methods of nano-titania mainly include gas-phase method and liquid-phase method.
- the gas phase method is a method of directly using gas or changing substances into gases by various means, making them undergo physical or chemical changes in the gaseous state, and finally condensing and growing to form nanoparticles during the cooling process.
- the gas phase method mainly includes gas condensation method, sputtering method, active hydrogen-molten metal reaction method, vacuum evaporation method on flowing liquid surface, mixed plasma method and electric heating evaporation method.
- the gas phase method usually has high reaction temperature, complex process technology, high requirements on equipment and technology, and large investment, so the product cost is high.
- the liquid-phase synthesis method Compared with the gas-phase synthesis method, the liquid-phase synthesis method has the advantages of easy reaction control, simple equipment and less energy consumption, and is widely used in the laboratory and industry to prepare titanium dioxide materials.
- Liquid phase methods mainly include precipitation method, hydrothermal method, sol-gel method, microemulsion method, hydrolysis method, etc.
- the nano-titania materials obtained by these methods have low yields, generally non-uniform particle size distribution, and long process flow.
- nano-TiO2 powders on the market are large particles formed by agglomeration of nano-scale particles, not nano-TiO2 materials in the true sense. These materials have poor dispersibility in water, are opaque, It is easy to settle, resulting in great defects in practical applications; at the same time, the price of nano-titanium dioxide materials is generally high, and its price is tens to hundreds of times that of micron and sub-micron titanium dioxide materials.
- the invention provides a steam bath method to obtain nano-titanium dioxide materials.
- the present invention adopts the following technical solutions:
- a device for preparing monodisperse nano-titania by a steam bath method the steam is provided by a mixed steam of hydrochloric acid and water formed by heating a hydrochloric acid solution; the steam pressure is greater than one atmospheric pressure; the device comprises:
- the container A and the container B are located in the sealed reaction kettle; the container A is used to place the solid powder of titanium oxide compound; the container B is used to place the hydrochloric acid solution; the container B is connected with the interior of the sealed reaction kettle.
- the steam outlet; the container A has a steam inlet communicated with the inside of the sealed reaction kettle.
- the container A and the container B are placed in an orderly manner in the sealed reactor according to a vertical direction, a horizontal direction or a combination of vertical and horizontal directions.
- the orderly arrangement is that the container A and the container B are arranged alternately.
- the container A is a mesh container; the mesh holes of the container A form the steam inlet, and the mesh hole density of the container A is above 80 mesh;
- the steam outlet of B is located at the upper end in the direction of gravity.
- the container A is a sieve container with a mesh size of 80 or more, wherein the steam penetrates into A through the mesh holes, so that the steam can better enter into contact with the surface of the titanium oxide compound, A thin aqueous layer was formed and the reaction started to form the product, which was still in Vessel A.
- the material of the container A is an inert material, preferably a PTFE corrosion-resistant material.
- the container B is preferably made of corrosion-resistant material, such as glass. Both the container A and the container B in FIG. 1 are accommodating trough-like structures. The upward opening of container A is used to put in the solid powder of titanium oxide compound.
- Containers A and B can be alternately spaced along the direction of gravity; containers A and B are alternately arranged up and down.
- the uppermost container is preferably container A
- the lowermost container is preferably container B.
- the steam inlet (grid port) of the container A faces the container B below, so that the steam of hydrochloric acid and water emitted in the container B is input.
- the steam outlet of the container B is open upward, and the steam outlet faces the container A.
- container A and container B are cylindrical containers or bottle-shaped containers with open upper ends and closed lower ends, and the peripheral side wall and bottom wall of container A are also sieve-like structures, so that The steam gets better into contact with the surface of the titanium oxide compound, forming a thin layer of water, and the reaction begins to form the product, which is still in vessel A.
- Both container A and container B are open to the top, the upper opening of container B forms a steam outlet, and a steam atmosphere is formed in the sealed reaction kettle, and then container A is placed in the whole steam atmosphere, and the sieve structure is used to fully contact the steam to form the target product.
- the titanium oxide solid powder includes one or a combination of nano-titanium dioxide, low-crystalline titanium dioxide, amorphous titanium dioxide, titanic acid, and titanium hydroxide.
- the titanium oxy compound solid powder is obtained from a titanium source after hydrolysis, separation, purification and drying; the titanium source is selected from titanium sulfate, titanium oxysulfate, titanium tetrachloride, and trichloride One or a combination of titanium oxide, titanium isopropoxide, tetrabutyl titanate, titanium alkoxide, fluorotitanic acid, and titanium tetrafluoride.
- the mass fraction of hydrochloric acid in the hydrochloric acid solution is 5% to 36%; the preferred mass fraction is 10% to 30%.
- the monodisperse nano-titanium dioxide is crystalline nano-scale titanium dioxide particles or agglomerates of crystalline nano-scale titanium dioxide particles; the surface of the nano-titanium dioxide material is acidic; the nano-titanium dioxide material does not contain organic matter.
- the monodisperse nano-titania is a colloidal nano-titania particle solution that can be spontaneously dispersed in water to form a long-term stable; the spontaneous dispersion process does not contain additives or dispersants.
- a method for preparing monodisperse nano titanium dioxide adopts steam bath method to prepare monodisperse nano titanium dioxide material; the method comprises the following steps:
- the container A and the container B are placed in the sealed reactor; wherein, the container B has a steam outlet communicating with the inside of the sealed reactor; the container A has a steam inlet communicated with the inside of the sealed reactor ;
- the sealed reaction kettle is placed in an oven, and the temperature in the oven is set to 100 degrees Celsius to 200 degrees Celsius; the hydrochloric acid solution forms a vapor pressure greater than one atmosphere in the sealed reaction kettle.
- the synthesized titanium dioxide nanoparticles have uniform size, and the particle size and crystal phase are controllable.
- the synthesized titanium dioxide material can be spontaneously dispersed when mixed with water to form an aqueous dispersion in which nano titanium dioxide particles are stably suspended.
- the titanium dioxide photocatalyst has excellent photocatalytic activity, and the catalytic efficiency is 10 times that of the P25 material.
- Fig. 1 is the schematic diagram of the preparation device of monodisperse nano titanium dioxide in the embodiment 1 of the present invention
- Fig. 2 is the schematic diagram of the preparation device of monodisperse titanium dioxide in Example 2 of the present invention.
- Fig. 3 is that the product obtained in Example 1 is dripped on the copper mesh after being dispersed in water, and the transmission electron microscope image obtained after drying is observed;
- Fig. 4 is the X-ray diffraction pattern of the titanium dioxide product prepared in Example 1, and the main crystal phase is anatase phase;
- Fig. 5 is the water dispersion liquid that the mass fraction obtained after adding water to the nano titanium dioxide product obtained in Example 1 is 5/1000; has a stable colloidal dispersion state;
- Example 6 is a graph showing the formaldehyde removal effect of the nano-titania product obtained in Example 1 and P25.
- a small amount of the product obtained in this example was dispersed in deionized water, and then a small amount was dripped onto a copper mesh, dried naturally, and used to observe the morphology of the sample with a transmission electron microscope, as shown in Figure 3. It can be seen from FIG. 3 that the particle size of the product titanium dioxide nanoparticles is 3 nanometers to 10 nanometers, which further indicates that the nano titanium dioxide obtained in this example has a small particle size and good monodispersity.
- Figure 4 is the X-ray diffraction pattern of the titanium dioxide product prepared in this example. It can be seen from Figure 4 that the main crystal phase of the nano-titanium dioxide obtained in this example is anatase phase, which has good crystallinity.
- the nano-titanium dioxide product obtained in this example is added to pure water, and a nano-titanium dioxide dispersion liquid with a mass fraction of 5/1000 can be spontaneously formed without stirring, and the dispersion liquid has good monodispersity.
- the aqueous dispersion is a stable colloidal dispersion, which can actually produce an obvious Tyndall phenomenon under the irradiation of light.
- the nanoparticles in the dispersion are stably suspended, do not agglomerate and are not easy to settle, and no obvious stratification occurs after 12 months of placement.
- the nano-titanium dioxide aqueous dispersion with a mass fraction of 5/10,000 obtained in this example can completely absorb ultraviolet light less than 370 nanometers in a 1 cm thick quartz cuvette, and the ultraviolet absorption ability is strong;
- the visible light region has extremely high light transmittance, and the transmittance is greater than 95%, which greatly expands the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
- the nano-titanium dioxide material obtained in this example also has excellent formaldehyde removal effect.
- the specific test method is as follows: spray 50 ml of this example with a concentration of 1% on a paper base of 1 square meter. Then, put the above paper base into a test chamber with a volume of 1 cubic meter, introduce a certain concentration and volume of formaldehyde, turn on the fan, and mix the air in the chamber evenly; then turn on the simulated sunlight Lights, and sample the formaldehyde concentration in the cabin air at regular intervals.
- This test uses P25 material as a control test.
- the particle size of the product titanium dioxide nanoparticles is 5 nanometers to 15 nanometers. , and further illustrate that the nano-titanium dioxide obtained in this example has a small particle size and good monodispersity.
- X-ray diffraction confirms that the main crystal phase of the nano-titania obtained in this example is anatase phase, which has good crystallinity.
- a small amount of the nano-titanium dioxide product obtained in this example is added to pure water, and a nano-titanium dioxide dispersion can be formed spontaneously without stirring.
- the dispersion has good monodispersity, and the aqueous dispersion is a stable colloidal dispersion. Under the irradiation of light, an obvious Tyndall phenomenon can be actually produced.
- the nanoparticles in the dispersion are stably suspended, do not agglomerate and are not easy to settle, and no obvious stratification occurs after being placed for 6 months.
- the nano-titanium dioxide aqueous dispersion with a mass fraction of 5/10,000 obtained in this example can completely absorb ultraviolet light less than 370 nanometers in a 1 cm thick quartz cuvette, and the ultraviolet absorption ability is strong;
- the visible light region has extremely high light transmittance, and the transmittance is greater than 90%, which greatly expands the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
- the nano-titanium dioxide material obtained in this example has excellent formaldehyde removal effect, and the formaldehyde removal rate within 12 hours is 94%.
- the specific test process is the same as that of Example 1.
- X-ray diffraction confirms that the main crystal phase of the nano-titania obtained in this example is rutile phase, which has good crystallinity.
- a small amount of the nano-titanium dioxide product obtained in this example is added to pure water, and a nano-titanium dioxide dispersion can be formed spontaneously without stirring.
- the dispersion has good monodispersity, and the aqueous dispersion is a stable colloidal dispersion. Under the irradiation of light, an obvious Tyndall phenomenon can be actually produced.
- the nanoparticles in the dispersion are stably suspended, do not agglomerate and are not easy to settle, and no obvious stratification occurs after being placed for 1 month.
- the nano-titanium dioxide aqueous dispersion with a mass fraction of 5/10,000 obtained in this example can completely absorb ultraviolet light less than 370 nanometers in a 1 cm thick quartz cuvette, and the ultraviolet absorption ability is strong;
- the visible light region has extremely high light transmittance, and the transmittance is greater than 80%, which greatly expands the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
- the particle size of the product titanium dioxide nanoparticles is 20 nanometers to 50 nanometers. , and further illustrate that the nano-titanium dioxide obtained in this example has a small particle size and good monodispersity.
- X-ray diffraction confirms that the main crystal phase of the nano-titania obtained in this example is anatase phase, contains a small amount of rutile phase, and the anatase phase has good crystallinity.
- a small amount of the nano-titanium dioxide product obtained in this example is added to pure water, and a nano-titanium dioxide dispersion can be formed spontaneously without stirring.
- the dispersion has good monodispersity, and the aqueous dispersion is a stable colloidal dispersion. Under the irradiation of light, an obvious Tyndall phenomenon can be actually produced.
- the nanoparticles in the dispersion are stably suspended, do not agglomerate and are not easy to settle, and no obvious stratification occurs after being placed for half a month.
- the nano-titanium dioxide aqueous dispersion with a mass fraction of 5/10,000 obtained in this example can completely absorb ultraviolet light less than 370 nanometers in a 1 cm thick quartz cuvette, and the ultraviolet absorption ability is strong;
- the visible light region has extremely high light transmittance, and the transmittance is greater than 60%, which expands the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
- the nano-titanium dioxide material obtained in this example has excellent formaldehyde removal effect, and the formaldehyde removal rate within 12 hours is 88%.
- the specific test process is the same as that of Example 1.
- the particle size of the product titanium dioxide nanoparticles is 15 nanometers to 30 nanometers. , and further illustrate that the nano-titanium dioxide obtained in this example has a small particle size and good monodispersity.
- X-ray diffraction confirms that the main crystal phase of the nano-titania obtained in this example is anatase phase, contains a small amount of rutile phase, and the anatase phase has good crystallinity.
- a small amount of the nano-titanium dioxide product obtained in this example is added to pure water, and a nano-titanium dioxide dispersion can be formed spontaneously without stirring.
- the dispersion has good monodispersity, and the aqueous dispersion is a stable colloidal dispersion. Under the irradiation of light, an obvious Tyndall phenomenon can be actually produced.
- the nanoparticles in the dispersion are stably suspended, do not agglomerate and are not easy to settle, and no obvious stratification occurs after being placed for 3 months.
- the nano-titanium dioxide aqueous dispersion with a mass fraction of 5/10,000 obtained in this example can completely absorb ultraviolet light less than 370 nanometers in a 1 cm thick quartz cuvette, and the ultraviolet absorption ability is strong;
- the visible light region has extremely high light transmittance, and the transmittance is greater than 80%, which expands the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
- the nano-titanium dioxide material obtained in this example has excellent formaldehyde removal effect, and the formaldehyde removal rate within 12 hours is 92%.
- the specific test process is the same as that of Example 1.
- the particle size of the product titanium dioxide nanoparticles is 30 nanometers to 50 nanometers. , and further illustrate that the nano-titanium dioxide obtained in this example has better monodispersity.
- X-ray diffraction confirms that the main crystal phase of the nano-titania obtained in this example is anatase phase, contains a small amount of rutile phase, and the anatase phase has good crystallinity.
- a small amount of the nano-titanium dioxide product obtained in this example is added to pure water, and a nano-titanium dioxide dispersion can be formed spontaneously without stirring.
- the dispersion has good monodispersity, and the aqueous dispersion is a stable colloidal dispersion. Under the irradiation of light, an obvious Tyndall phenomenon can be actually produced.
- the nanoparticles in the dispersion are stably suspended, do not agglomerate and are not easy to settle, and no obvious stratification occurs after being placed for 2 months.
- the nano-titanium dioxide aqueous dispersion with a mass fraction of 5/10,000 obtained in this example can completely absorb ultraviolet light less than 370 nanometers in a 1 cm thick quartz cuvette, and the ultraviolet absorption ability is strong;
- the visible light region has extremely high light transmittance, and the light transmittance is greater than 70%, which expands the application of titanium dioxide materials in the fields of ultraviolet absorption, aesthetics and other products.
- the nano-titanium dioxide material obtained in this example has excellent formaldehyde removal effect, and the formaldehyde removal rate within 12 hours is 83%.
- the specific test process is the same as that of Example 1.
- any numerical value recited herein includes all values of the lower value and the upper value in one unit increments from the lower value to the upper value, where there is an interval of at least two units between any lower value and any higher value, i.e. Can.
- the number of components or process variables eg, temperature, pressure, time, etc.
- the intent is to illustrate that the The specification also explicitly lists values such as 15 to 85, 22 to 68, 43 to 51, 30 to 32, and the like.
- one unit is appropriately considered to be 0.0001, 0.001, 0.01, 0.1.
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Abstract
L'invention concerne une méthode et un dispositif de préparation de dioxyde de titane nanométrique monodispersé, au moyen desquels un nanomatériau de dioxyde de titane présentant d'excellentes performances peut être développé à faible coût et à grande échelle. L'invention concerne un dispositif de préparation de dioxyde de titane nanométrique monodispersé à l'aide d'un procédé à bain de vapeur, dans lequel la vapeur est fournie au moyen d'une vapeur mixte d'acide chlorhydrique et d'eau formée par chauffage d'une solution d'acide chlorhydrique, et la pression de vapeur est supérieure à une atmosphère. Le dispositif comprend une cuve de réaction hermétiquement scellée placée dans un environnement de 100°C à 200°C, et un récipient A et un récipient B situés dans la cuve de réaction scellée, le récipient A étant utilisé pour contenir une poudre d'oxyde de titane solide ; le récipient B étant utilisé pour contenir la solution d'acide chlorhydrique; le récipient B ayant une sortie de vapeur en communication avec l'intérieur de la cuve de réaction hermétiquement scellée; et le récipient A ayant une entrée de vapeur en communication avec l'intérieur de la cuve de réaction hermétiquement scellée.
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CN1328962A (zh) * | 2000-06-15 | 2002-01-02 | 泰兴纳米材料厂 | 一种制备纳米二氧化钛微粉的方法 |
US20080064592A1 (en) * | 2004-10-14 | 2008-03-13 | Insoo Kim | Method for Synthesizing Nano-Sized Titanium Dioxide Particles |
CN102502520A (zh) * | 2011-10-28 | 2012-06-20 | 泉州师范学院 | 一种制备水合氧化物的高温蒸汽热解法及其应用 |
CN102616842A (zh) * | 2012-04-01 | 2012-08-01 | 攀枝花新中钛科技有限公司 | 一种制备钛白粉的方法 |
CN203159246U (zh) * | 2013-01-23 | 2013-08-28 | 自贡市亚钛化工科技有限公司 | 一种生产钛黄粉使用的浸取球 |
CN110065967A (zh) * | 2019-04-10 | 2019-07-30 | 浙江迈实科技有限公司 | 一种纳米级二氧化钛制备方法 |
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JP2000262891A (ja) * | 1999-03-16 | 2000-09-26 | Kuraray Chem Corp | 悪臭ガス吸着剤及びその製造方法 |
KR20010025629A (ko) * | 2001-01-12 | 2001-04-06 | 이종국 | 산처리에 의한 산화티탄 결정분말의 제조 |
CN101805529A (zh) * | 2009-02-17 | 2010-08-18 | 中国科学院理化技术研究所 | 染料敏化太阳能电池用纳米二氧化钛浆料的制备方法 |
CN101830502B (zh) * | 2010-03-19 | 2012-05-02 | 浙江大学 | 一种单分散二氧化钛纳米微球及其制备方法 |
CN108821337B (zh) * | 2018-06-21 | 2021-01-12 | 方嘉城 | 一种纳米二氧化钛的制备方法 |
CN110790306B (zh) * | 2018-08-01 | 2020-12-11 | 北京化工大学 | 单分散锐钛矿纳米二氧化钛透明液相分散体的制备方法 |
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CN1328962A (zh) * | 2000-06-15 | 2002-01-02 | 泰兴纳米材料厂 | 一种制备纳米二氧化钛微粉的方法 |
US20080064592A1 (en) * | 2004-10-14 | 2008-03-13 | Insoo Kim | Method for Synthesizing Nano-Sized Titanium Dioxide Particles |
CN102502520A (zh) * | 2011-10-28 | 2012-06-20 | 泉州师范学院 | 一种制备水合氧化物的高温蒸汽热解法及其应用 |
CN102616842A (zh) * | 2012-04-01 | 2012-08-01 | 攀枝花新中钛科技有限公司 | 一种制备钛白粉的方法 |
CN203159246U (zh) * | 2013-01-23 | 2013-08-28 | 自贡市亚钛化工科技有限公司 | 一种生产钛黄粉使用的浸取球 |
CN110065967A (zh) * | 2019-04-10 | 2019-07-30 | 浙江迈实科技有限公司 | 一种纳米级二氧化钛制备方法 |
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