CN113896231B - Preparation method of titanium dioxide material - Google Patents
Preparation method of titanium dioxide material Download PDFInfo
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- CN113896231B CN113896231B CN202110361403.9A CN202110361403A CN113896231B CN 113896231 B CN113896231 B CN 113896231B CN 202110361403 A CN202110361403 A CN 202110361403A CN 113896231 B CN113896231 B CN 113896231B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000000463 material Substances 0.000 title claims abstract description 51
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000007787 solid Substances 0.000 claims abstract description 53
- 150000001875 compounds Chemical class 0.000 claims abstract description 48
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims description 42
- 239000010936 titanium Substances 0.000 claims description 33
- 229910052719 titanium Inorganic materials 0.000 claims description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 18
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 17
- 239000000460 chlorine Substances 0.000 claims description 17
- 229910052801 chlorine Inorganic materials 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- -1 titanium alkoxide Chemical class 0.000 claims description 4
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 3
- 239000000047 product Substances 0.000 description 90
- 239000006185 dispersion Substances 0.000 description 40
- 239000012071 phase Substances 0.000 description 23
- 239000002105 nanoparticle Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 239000010703 silicon Substances 0.000 description 12
- 239000003973 paint Substances 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 230000031700 light absorption Effects 0.000 description 10
- 239000002243 precursor Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 10
- 239000008213 purified water Substances 0.000 description 8
- 238000007789 sealing Methods 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 7
- 241000519995 Stachys sylvatica Species 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 230000037072 sun protection Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000002269 spontaneous effect Effects 0.000 description 4
- 238000001246 colloidal dispersion Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 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 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 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 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000010985 leather Substances 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
- KELHQGOVULCJSG-UHFFFAOYSA-N n,n-dimethyl-1-(5-methylfuran-2-yl)ethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=C(C)O1 KELHQGOVULCJSG-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- 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
- 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
-
- B01J35/39—
-
- 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
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- 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
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The application provides a preparation method of a titanium dioxide material, which comprises the following steps: (1) preparing a titanyl chloride solid powder compound; (2) Controlling the water content of the titanyl chloride solid powder compound in the step (1) to be one to fifty percent by mass of water; preferably, the mass fraction of water is five to thirty percent; (3) And (3) heating the titanium oxychloride solid powder compound in the step (2) at a low temperature in a closed environment to obtain the titanium dioxide material. The preparation method of the nano titanium dioxide material can develop the nano titanium dioxide material with low cost and high performance on a large scale.
Description
Technical Field
The application particularly relates to a preparation method of a titanium dioxide material.
Background
The nano titanium dioxide is titanium dioxide with the particle size smaller than 100 nanometers, has special effects of small particle size, high specific surface area, excellent photocatalytic activity, stable chemical and thermal properties, super-affinity and the like, and has irreplaceable application advantages in the fields of air treatment, sterilization and disinfection, self-cleaning materials, sun-screening skin care products and the like.
At present, the preparation modes of nano titanium dioxide can be divided into two major categories of physical methods and chemical methods. The physical method is to control the grain size and crystal form only by physical mechanics or solid phase re-separation, and the chemical composition of the prepared powder is not changed before and after the powder is prepared, and the common method is a gas phase condensation method and a crushing method. The gas-phase condensation method is not suitable for preparing high-melting-point and high-boiling-point oxides, and the crushing method utilizes huge energy of mechanical rotation and vibration to crush raw materials into nano-scale particles, so that the obtained powder is irregular in shape, the particle size distribution is wide, and uniform nano powder is difficult to obtain.
Chemical methods can be classified into solid phase methods, gas phase methods and liquid phase methods according to the morphology of the reactant system. Wherein the solid phase method is not suitable for the preparation of nanoparticles because the reaction only occurs between solid particles, and the mixing degree between solids is very uneven. The gas phase method is a method of changing a substance into a gas directly by using the gas or by various means to make the substance physically or chemically change in the gas state, and finally condensing and growing to form nano particles in the cooling process. The gas phase method mainly comprises a gas condensation method, a sputtering method, an active hydrogen-molten metal reaction method, a flowing liquid surface vacuum evaporation method, a mixed plasma method, an electrified heating evaporation method and the like. The gas phase method has high reaction temperature, complex process technology, high requirements on equipment and technology, large investment and high product cost. The liquid phase synthesis method has the advantages of easy control of reaction, simple equipment, low energy consumption and the like, and is a method for preparing titanium dioxide materials widely adopted in the laboratory and industry. The liquid phase method mainly comprises precipitation method, hydrothermal method, sol-gel method, microemulsion method, hydrolysis method, etc. The nano titanium dioxide material obtained by the method has low yield, generally uneven particle size distribution and longer process flow.
The nano titanium dioxide powder is large particles formed by agglomeration of nano particles in the current market, which are not nano titanium dioxide materials in the true sense, and the materials have poor dispersibility in water, are opaque and are easy to settle, so that the materials have great defects in practical application; meanwhile, the price of the nano titanium dioxide material is generally higher, and the price of the nano titanium dioxide material is tens to hundreds times of that of the micron and submicron titanium dioxide material. Therefore, developed countries such as the united states, japan, europe and the like have been actively studied on nano titanium dioxide, and a lot of manpower and material resources have been put into front and rear, but nano titanium dioxide materials excellent in performance have not been developed on a large scale at low cost.
Disclosure of Invention
In view of the above-mentioned shortcomings, it is an object of the present application to provide a method for preparing a nano titania material, which can develop a low-cost and high-performance nano titania material on a large scale.
The technical method adopts titanium oxychloride solid powder as a precursor, controls the diffusion path of solute in the conversion process by controlling the water content of the material, and finally obtains a nano material product with small scale, uniform particle size and single dispersion.
In order to achieve the above purpose, the application adopts the following technical scheme:
a preparation method of a titanium dioxide material comprises the following steps:
(1) Preparing a titanium oxychloride solid powder compound;
(2) Controlling the water content of the titanium oxychloride solid powder compound in the step 1 to be one percent to fifty percent by mass of water; the preferred water mass fraction is five to thirty percent.
(3) And (3) heating the titanium oxychloride solid powder compound in the step (2) at a low temperature in a closed environment to obtain the titanium dioxide material.
As a preferred embodiment, the titanium dioxide material is a colloidal solution which can spontaneously disperse in water to form stable suspension of nano titanium dioxide particles; the nano titanium dioxide particles are crystalline nano titanium dioxide particles.
As a preferred embodiment, the titanyl chloride solid powder compound has the chemical formula TiOxCly; the x value is from 1.7 to 2.3; the y value is 0.01 to 0.5.
As a preferred embodiment, the titanyl chloride solid powder compound in step 1 may further contain hydrogen; the number ratio of the contained hydrogen to the titanium is 1:100 to 1:10.
As a preferred embodiment, the titanium oxychloride solid powder compound in step 1 has a number ratio of oxygen to titanium of 1.8 to 2.2.
As a preferred embodiment, the titanium oxychloride solid powder compound in the step 1 has a chlorine to titanium number ratio of 0.03 to 0.2.
As a preferred embodiment, the low temperature heating in step 3 is at a temperature of 100 degrees celsius to 200 degrees celsius; the duration of the low temperature heating is 2 hours to 24 hours.
As a preferred embodiment, the preparation of the titanyl chloride solid powder compound in step 1 is obtained after contacting titanium chloride with water or water vapor; the titanium chloride is selected from one or a combination of a plurality of titanium tetrachloride, titanium tetrachloride aqueous solution, titanium trichloride and titanium dichloride.
As a preferred embodiment, the preparation of the titanyl chloride solid powder compound described in step 1 is obtained by direct hydrolysis of a titanium alkoxide in an aqueous solution containing hydrochloric acid.
As a preferred embodiment, the preparation of the titanyl chloride solid powder compound in step 1 is obtained by reacting a titanium oxide compound with one or a combination of hydrochloric acid, hydrochloric acid solution, chlorine gas solution; the titanium oxide compound is selected from one or a combination of a plurality of low-crystallinity titanium dioxide, amorphous titanium dioxide, titanic acid, titanium suboxide, titanium monoxide, metatitanic acid, titanium hydroxide and hydrated titanic acid.
The application has the advantages that:
1. the technology has universality, low price and simple process, and can be applied to large-scale synthesis.
2. The synthesized titanium dioxide particles have uniform size and controllable particle size, and can be spontaneously dispersed in water to form a colloid solution with stable suspension of nano titanium dioxide particles.
3. The titanium dioxide photocatalyst has excellent photocatalytic activity.
Specific embodiments of the application are disclosed in detail below with reference to the following description and drawings, indicating the manner in which the principles of the application may be employed. It should be understood that the embodiments of the application are not limited in scope thereby.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used herein is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the application, and that other drawings can be obtained from these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a scanning electron microscope image obtained by dispersing the product obtained in example 1 with water, then dripping the product on a silicon wafer, drying and then observing the product;
FIG. 2 is an X-ray diffraction pattern of the titanium dioxide product prepared in example 1, the primary crystalline phase being the rutile phase;
FIG. 3 is a graph showing the stable colloidal dispersion of an aqueous dispersion of one thousandth of the weight of the nano-titania product obtained in example 1 after adding water;
FIG. 4 is a scanning electron microscope image obtained by dispersing the product obtained in example 4 with water, then dripping the product on a silicon wafer, drying and then observing the product;
FIG. 5 is a scanning electron micrograph of the product obtained in comparative example 1, which is a petal-like large particle agglomerate.
Detailed Description
In order to make the technical solution of the present application better understood by those skilled in the art, the technical solution of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, shall fall within the scope of the application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Example 1
Slowly dripping 10 g of titanium tetrachloride liquid into 200 ml of water, continuously stirring for 7 days after dripping to obtain white precipitate, centrifuging, and drying at normal temperature to obtain a titanium oxychloride solid powder compound; measuring and controlling the water content in the titanyl chloride solid powder compound to be twenty percent; subsequently, the powder is put into a reaction kettle for sealing, and then is put into an oven for heating for 20 hours at 140 ℃ to obtain a titanium dioxide product. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium, oxygen and chlorine are determined by energy spectrum; wherein the ratio of oxygen to titanium is about 2.1 and the ratio of chlorine to titanium is about 0.16.
A small amount of the product obtained in the embodiment 1 is dispersed in deionized water, then a small amount of the product is dripped on a silicon wafer, the silicon wafer is naturally dried, and the dried silicon wafer is adhered to a sample stage of a scanning electron microscope by using conductive adhesive and is used for observing the appearance of the sample by the scanning electron microscope, as shown in figure 1. From fig. 1, it can be seen that the titanium dioxide nanoparticle is in the shape of a nano rod, the length of the particle is 50-100 nanometers, the particle diameter of the particle is mainly 15-20 nanometers, and the uniformity is good. Fig. 2 is an X-ray diffraction chart of the titanium dioxide product prepared in example 1, and it can be seen from fig. 2 that the crystalline phase of the nano titanium dioxide prepared in example 1 is rutile phase and has good crystallinity.
The nano titanium dioxide product obtained in the embodiment 1 is added into water to obtain nano titanium dioxide dispersion liquid with the mass fraction of one thousandth, and as shown in fig. 3, the dispersion liquid has good monodispersity, can form stable colloidal dispersion liquid in aqueous solution, has stable nanoparticle suspension, is not agglomerated and is not easy to settle, and the solution is not layered after being placed for 3 months. The nano titanium dioxide obtained in example 1 was dispersed in water to form an aqueous dispersion with a concentration of five parts per million, and then the dispersion was placed in a quartz cuvette with a thickness of 1 cm to test the ultraviolet-visible light absorption curve of the sample. The dispersion can completely absorb ultraviolet light smaller than 380 nanometers, has strong ultraviolet light absorption capacity, and has good light transmittance in a visible light region larger than 400 nanometers, wherein the light transmittance is larger than sixty percent. Compared with the P25 nano titanium dioxide material, the transparency of the product obtained by the embodiment is improved by 40 times by taking 550 nano wavelength as an example, and the adding application of the titanium dioxide material in the product fields of ultraviolet absorption, attractive appearance and the like is greatly expanded, such as developing transparent paint for doors and windows, leather products, glass, mirrors and the like without forming white spots, developing skin care and sun protection products with transparent and natural complexion, developing transparent film products, transparent durable finishing paint, products of fine ceramics and the like. In summary, the application has the advantages that: (1) The technology has universality, low price and simple process, and can be applied to large-scale synthesis. (2) The synthesized titanium dioxide particles have uniform size and controllable particle size, and can be spontaneously dispersed in water to form a colloid solution with stable suspension of nano titanium dioxide particles. (3) The dispersion liquid of the product has extremely high transparency, can be used for developing transparent coating products, such as spraying on the surfaces of doors and windows, leathers, glass, mirrors and the like, and does not form white spots; can also be used for manufacturing transparent and natural skin-care and sun-protection products; and is also beneficial to developing products such as transparent film products, transparent durable finish paint, fine ceramics and the like.
Example 2
Slowly dripping 10 g of titanium trichloride liquid into 100 ml of water, heating to 50 ℃ after dripping, continuously stirring for 6 hours to obtain white precipitate, centrifuging, and drying at 60 ℃ to obtain a titanium oxychloride solid powder compound; measuring and controlling the water content in the titanyl chloride solid powder compound to be ten percent; subsequently, the powder is put into a reaction kettle for sealing, and then is put into an oven for heating for 8 hours at 180 ℃ to obtain a titanium dioxide product. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium, oxygen and chlorine are determined by energy spectrum; wherein the ratio of oxygen to titanium is about 1.9 and the ratio of chlorine to titanium is about 0.1.
A small amount of the product obtained in the embodiment 2 is dispersed in deionized water, and then a small amount of the product is dripped on a silicon wafer for observing the appearance of a sample by a scanning electron microscope, so that the titanium dioxide nano particles are in a nano rod shape, the length of the particles is 60-150 nanometers, the particle size of the particles is mainly 20-30 nanometers, and the uniformity is good. The X-ray diffraction confirmed that the main crystal phase of the nano titanium dioxide obtained in the present example 2 was a rutile phase having good crystallinity.
When a small amount of the titanium dioxide material product obtained in the embodiment 2 is put into purified water, spontaneous dissolution and dispersion of the titanium dioxide material product in the purified water can be seen, a colloidal aqueous dispersion with stable suspension of nano titanium dioxide particles is formed, the nano particles in the dispersion are stable in suspension and do not agglomerate, the obvious tyndall phenomenon is achieved, and the obvious layering phenomenon does not occur even when the dispersion is placed for half a month. The nano titanium dioxide obtained in example 2 was dispersed in water to form an aqueous dispersion with a concentration of five parts per million, and then the dispersion was placed in a quartz cuvette with a thickness of 1 cm to test the ultraviolet-visible light absorption curve of the sample. The dispersion can completely absorb ultraviolet light smaller than 380 nanometers, has strong ultraviolet light absorption capacity, and has good light transmittance in a visible light region larger than 400 nanometers, wherein the light transmittance is more than thirty percent. Compared with the P25 nano titanium dioxide material, the transparency of the product obtained by the embodiment is improved by 20 times by taking 550 nano wavelength as an example, and the adding application of the titanium dioxide material in the product fields of ultraviolet absorption, attractive appearance and the like is expanded, such as developing transparent paint for doors and windows, leathers, glass, mirrors and the like without forming white spots, developing skin care and sun protection products with transparent and natural complexion, developing transparent film products, transparent durable finishing paint, products of fine ceramics and the like.
Example 3
Mixing water vapor and titanium dichloride gas according to the mass ratio of water to titanium dichloride of 20:1 to form white precipitate, centrifugally separating, and drying at normal temperature to obtain a titanium oxychloride solid powder compound; measuring and controlling the water content in the titanium oxychloride solid powder compound to be fifty percent; and then, placing the powder into a reaction kettle for sealing, and then placing the powder into a microwave oven for microwave heating at 160 ℃ for 3 hours to obtain a titanium dioxide product. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium, oxygen and chlorine are determined by energy spectrum; wherein the ratio of oxygen to titanium is about 1.8 and the ratio of chlorine to titanium is about 0.2.
A small amount of the product obtained in the embodiment 3 is dispersed in deionized water, and then a small amount of the product is dripped on a silicon wafer for observing the appearance of a sample by a scanning electron microscope, so that the titanium dioxide nano particles are in a nano rod shape, the length of the particles is 100-200 nanometers, the particle size of the particles is mainly 15-20 nanometers, and the uniformity is good. The X-ray diffraction confirmed that the main crystal phase of the nano titanium dioxide obtained in the present example 2 was a rutile phase having good crystallinity.
When a small amount of the titanium dioxide material product obtained in the embodiment 3 is put into purified water, spontaneous dissolution and dispersion of the titanium dioxide material product in the purified water can be seen, a colloidal aqueous dispersion with stable suspension of nano titanium dioxide particles is formed, the nano particles in the dispersion are stable in suspension and do not agglomerate, the obvious tyndall phenomenon is achieved, and the obvious layering phenomenon does not occur after the dispersion is placed for 1 month. The nano titanium dioxide obtained in example 3 was dispersed in water to form an aqueous dispersion with a concentration of five parts per million, and then the dispersion was placed in a quartz cuvette with a thickness of 1 cm to test the ultraviolet-visible light absorption curve of the sample. The dispersion can completely absorb ultraviolet light smaller than 380 nanometers, has strong ultraviolet light absorption capacity, and has good light transmittance in a visible light region larger than 400 nanometers, wherein the light transmittance is larger than forty percent. Compared with the P25 nano titanium dioxide material, the transparency of the product obtained by the embodiment is improved by 30 times by taking 550 nano wavelength as an example, and the adding application of the titanium dioxide material in the product fields of ultraviolet absorption, attractive appearance and the like is expanded, such as developing transparent paint for doors and windows, leathers, glass, mirrors and the like without forming white spots, developing skin care and sun protection products with transparent and natural complexion, developing transparent film products, transparent durable finishing paint, products of fine ceramics and the like.
Example 4
Slowly dropwise adding 10 g of tetrabutyl titanate into 200 ml of hydrochloric acid aqueous solution with the concentration of 1 mol per liter under stirring, continuously stirring for 2 hours after dropwise adding to obtain white precipitate, centrifuging, and drying at normal temperature to obtain a titanium oxychloride solid powder compound; measuring and controlling the water content in the titanyl chloride solid powder compound to be forty percent; subsequently, the powder is put into a reaction kettle for sealing, and then is put into an oven for heating at 120 ℃ for 24 hours, so as to obtain a titanium dioxide product.
After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components are titanium, oxygen and chlorine by energy spectrum measurement; wherein the ratio of oxygen to titanium is about 1.8 and the ratio of chlorine to titanium is about 0.18.
A small amount of the product obtained in the example 4 is dispersed in deionized water, then a small amount of the product is dripped on a silicon wafer, the silicon wafer is naturally dried, and the dried silicon wafer is adhered to a sample stage of a scanning electron microscope by using conductive adhesive and is used for observing the appearance of the sample by the scanning electron microscope, as shown in fig. 4. From fig. 4, it can be seen that the particle size of the product titanium dioxide nanoparticle is 5 nm to 10 nm, so that it is further illustrated that the titanium dioxide nanoparticle obtained in this embodiment has a small particle size and better monodispersity.
The nano titanium dioxide prepared by the embodiment has the main crystal phase of anatase phase and better crystallinity. The nano titanium dioxide product obtained in the embodiment is added into water to obtain nano titanium dioxide dispersion liquid with the mass fraction of five thousandths, the dispersion liquid has good monodispersity, stable colloidal dispersion liquid can be formed in aqueous solution, nano particles are stable in suspension, do not agglomerate and are not easy to settle, and the solution is not layered after being placed for more than 6 months.
The nano titanium dioxide material obtained in this example has good photocatalytic activity, and the catalytic efficiency is 8 times that of commercial P25 material, and the specific comparison mode is that 2 g of the product obtained in this example 1 and a P25 (Degusa) sample are respectively weighed and dispersed in 100 ml of rhodamine B solution with the concentration of 2.0X10-5 mol/L, and the mixture is placed in a dark place and magnetically stirred for 30 minutes, so that the temperature balance and the adsorption balance are achieved. And then starting a simulated sunlight lamp, stirring, taking out 3 milliliters of samples at fixed time intervals, centrifugally separating particles, measuring the absorbance of the solution at 550 nanometers by using an ultraviolet-visible spectrometer, and calculating the residual concentration of rhodamine B.
Example 5
Slowly dripping 10 g of titanium isopropoxide into 200 ml of hydrochloric acid aqueous solution with the concentration of 0.5 mol per liter under stirring, continuously stirring for 2 hours after dripping to obtain white precipitate, centrifuging, and drying at normal temperature to obtain a titanium oxychloride solid powder compound; measuring and controlling the water content in the titanium oxychloride solid powder compound to be thirty percent; subsequently, the powder was put into a reaction kettle for sealing, and then placed into an oil bath for heating at 160 ℃ for 20 hours, thereby obtaining a titanium dioxide product. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium, oxygen and chlorine are determined by energy spectrum; wherein the ratio of oxygen to titanium is about 2.0 and the ratio of chlorine to titanium is about 0.12.
A small amount of the product obtained in the embodiment 5 is taken to be dispersed in deionized water, and then a small amount of the product is taken to be dripped on a silicon wafer for observing the appearance of a sample by a scanning electron microscope, so that the particle size of the product titanium dioxide nano particles is 8-20 nanometers, and further the nano titanium dioxide obtained in the embodiment has small particle size and good monodispersity. The X-ray diffraction confirmed that the main crystal phase of the nano titania obtained in this example 5 was an anatase phase having good crystallinity.
When a small amount of the titanium dioxide material product obtained in the embodiment 5 is put into purified water, spontaneous dissolution and dispersion of the titanium dioxide material product in the purified water can be seen, a colloidal aqueous dispersion with stable suspension of nano titanium dioxide particles is formed, the nano particles in the dispersion are stable in suspension and do not agglomerate, the obvious tyndall phenomenon is achieved, and the obvious layering phenomenon does not occur after the dispersion is placed for 8 months. The nano titanium dioxide obtained in example 5 was dispersed in water to form an aqueous dispersion with a concentration of five parts per million, and then the dispersion was placed in a quartz cuvette with a thickness of 1 cm to test the ultraviolet-visible light absorption curve of the sample. The dispersion can completely absorb ultraviolet light smaller than 370 nanometers, has strong ultraviolet light absorption capacity, and has good light transmittance in a visible light region larger than 400 nanometers, wherein the light transmittance is larger than ninety percent. Compared with the P25 nano titanium dioxide material, the transparency of the product obtained by the embodiment is improved by 60 times by taking 550 nano wavelength as an example, and the adding application of the titanium dioxide material in the product fields of ultraviolet absorption, attractive appearance and the like is expanded, such as developing transparent paint for doors and windows, leathers, glass, mirrors and the like without forming white spots, developing skin care and sun protection products with transparent and natural complexion, developing transparent film products, transparent durable finishing paint, products of fine ceramics and the like.
The nano-titania material obtained in this example 5 has good photocatalytic activity, and the catalytic efficiency is 9 times that of the commercial P25 material, and the specific comparison manner is as described in example 4.
Example 6
Dispersing 2 g of metatitanic acid in 50 ml of hydrochloric acid aqueous solution with the concentration of 1 mol per liter, heating to 50 ℃ and continuously stirring for 24 hours, separating a product, and drying at 50 ℃ to obtain a titanyl chloride solid powder compound; measuring and controlling the water content in the titanium oxychloride solid powder compound to be thirty percent; and then, the powder is put into a reaction kettle for sealing, and then is put into a microwave oven for microwave heating at 140 ℃ for 5 hours, so that a titanium dioxide product is obtained. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium, oxygen and chlorine are determined by energy spectrum; wherein the ratio of oxygen to titanium is about 2.1 and the ratio of chlorine to titanium is about 0.14.
A small amount of the product obtained in the embodiment 6 is taken to be dispersed in deionized water, and then a small amount of the product is taken to be dripped on a silicon wafer for observing the appearance of a sample by a scanning electron microscope, so that the particle size of the titanium dioxide nanoparticle of the product is 20-50 nanometers, and further the nano titanium dioxide obtained in the embodiment has small particle size and better monodispersity. X-ray diffraction confirmed that the nano-titania obtained in example 6 had a main crystal phase of anatase phase having good crystallinity and contained a trace amount of rutile phase.
When a small amount of the titanium dioxide material product obtained in the embodiment 6 is put into purified water, spontaneous dissolution and dispersion of the titanium dioxide material product in the purified water can be seen, a colloidal aqueous dispersion with stable suspension of nano titanium dioxide particles is formed, the nano particles in the dispersion are stable in suspension and do not agglomerate, the obvious tyndall phenomenon is achieved, and the obvious layering phenomenon does not occur after the dispersion is placed for 3 months. The nano titanium dioxide obtained in example 6 was dispersed in water to form an aqueous dispersion with a concentration of five parts per million, and then the dispersion was placed in a quartz cuvette with a thickness of 1 cm to test the ultraviolet-visible light absorption curve of the sample. The dispersion can completely absorb ultraviolet light smaller than 370 nanometers, has strong ultraviolet light absorption capacity, and has good light transmittance in a visible light region larger than 400 nanometers, wherein the light transmittance is larger than seventy percent. Compared with the P25 nano titanium dioxide material, the transparency of the product obtained by the embodiment is improved by 45 times by taking 550 nano wavelength as an example, and the adding application of the titanium dioxide material in the product fields of ultraviolet absorption, attractive appearance and the like is expanded, such as developing transparent paint for doors and windows, leathers, glass, mirrors and the like without forming white spots, developing skin care and sun protection products with transparent and natural complexion, developing transparent film products, transparent durable finishing paint, products of fine ceramics and the like.
The nano-titania material obtained in this example 6 has good photocatalytic activity, and catalytic efficiency 7.3 times that of the commercial P25 material, and the specific comparison is as described in example 4.
Comparative example 1
Slowly dripping 10 g of titanium tetrachloride liquid into 200 ml of water, continuously stirring for 7 days after dripping to obtain white precipitate, centrifuging, and drying at normal temperature to obtain a titanium oxychloride solid powder compound; measuring and controlling the water content in the titanium oxychloride solid powder compound to be ninety percent to obtain slurry titanium oxychloride solid suspension; and then, the titanium oxychloride solid suspension is put into a reaction kettle for sealing, and then is put into an oven for heating for 20 hours at 140 ℃ to obtain a titanium dioxide product. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium, oxygen and chlorine are determined by energy spectrum; wherein the ratio of oxygen to titanium is about 2.1 and the ratio of chlorine to titanium is about 0.16. The product obtained in this comparative example contains a large number of petal-shaped large particles, as shown in scanning electron microscope fig. 5; meanwhile, the product cannot be dispersed in water to form stable and transparent dispersion liquid, the obtained product is suspension liquid, and precipitation delamination can occur within a few hours; in addition, the comparative product is rutile phase, and has poor photocatalytic performance. The comparative example cannot obtain the inventive effect of the product of the example in terms of product morphology, dispersibility, crystal phase, catalytic efficiency and other structures and performances.
Comparative example 2
Slowly dripping 10 g of titanium tetrachloride liquid into 200 ml of water, continuously stirring for 7 days after dripping to obtain white precipitate, centrifuging, washing for multiple times, and drying at normal temperature to obtain a titanium oxide solid powder compound; measuring and controlling the water content in the titanyl solid powder compound to be twenty percent; subsequently, the powder is put into a reaction kettle for sealing, and then is put into an oven for heating for 20 hours at 140 ℃ to obtain a titanium dioxide product. After the titanium oxychloride solid powder compound precursor is completely dried, under vacuum, the main components of the titanium oxychloride solid powder compound precursor are titanium and oxygen through energy spectrum measurement; wherein the ratio of oxygen to titanium is about 2.0 and the ratio of chlorine to titanium is less than 0.01. The product obtained in this comparative example contains a large number of large petal-like particles; meanwhile, the product cannot be dispersed in water to form stable and transparent dispersion liquid, and the obtained product is suspension liquid, so that precipitation delamination can occur within a few hours. The inventive effect of the product of the example cannot be obtained in terms of morphology, dispersibility and other structures and properties of the product.
Any numerical value recited herein includes all values of the lower and upper values that are incremented by one unit from the lower value to the upper value, as long as there is a separation of at least two units between any lower value and any higher value. For example, if it is stated that the number of components or the value of a process variable (e.g., temperature, pressure, time, etc.) is from 1 to 90, preferably from 20 to 80, more preferably from 30 to 70, then the purpose is to explicitly list such values as 15 to 85, 22 to 68, 43 to 51, 30 to 32, etc. in this specification as well. For values less than 1, one unit is suitably considered to be 0.0001, 0.001, 0.01, 0.1. These are merely examples that are intended to be explicitly recited in this description, and all possible combinations of values recited between the lowest value and the highest value are believed to be explicitly stated in the description in a similar manner.
Unless otherwise indicated, all ranges include endpoints and all numbers between endpoints. "about" or "approximately" as used with a range is applicable to both endpoints of the range. Thus, "about 20 to 30" is intended to cover "about 20 to about 30," including at least the indicated endpoints.
It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the present teachings should, therefore, be determined not with reference to the above description, but instead should be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are incorporated herein by reference for the purpose of completeness. The omission of any aspect of the subject matter disclosed herein in the preceding claims is not intended to forego such subject matter, nor should the inventors regard such subject matter as not be considered to be part of the disclosed subject matter.
Claims (2)
1. The preparation method of the titanium dioxide material is characterized by comprising the following steps:
(1) Preparing a titanium oxychloride solid powder compound; the chemical formula of the titanyl chloride solid powder compound is TiOxCly; wherein the y value is 0.01 to 0.5; the titanium oxychloride solid powder compound in step (1) has a number ratio of oxygen to titanium of 1.8 to 2.2; the titanium oxychloride solid powder compound in the step (1) also contains hydrogen; the titanium oxychloride solid powder compound contains hydrogen and titanium in a number ratio of 1:100 to 1:10; the titanium oxychloride solid powder compound in the step (1) has a chlorine to titanium number ratio of 0.03 to 0.2;
wherein, the preparation of the titanyl chloride solid powder compound in the step (1) is obtained by contacting titanium chloride with water or water vapor, and the titanium chloride is selected from one or a combination of a plurality of titanium tetrachloride, titanium trichloride and titanium dichloride; alternatively, the preparation of the titanyl chloride solid powder compound in step (1) is obtained by direct hydrolysis of a titanium alkoxide in an aqueous solution containing hydrochloric acid;
(2) Controlling the water content of the titanyl chloride solid powder compound in the step (1) to be one to fifty percent by mass of water;
(3) Heating the titanium oxychloride solid powder compound in the step (2) at a low temperature in a closed environment to obtain a titanium dioxide material; the low-temperature heating temperature in the step (3) is 100-200 ℃; the low-temperature heating time is 2 to 24 hours; the titanium dioxide material is a colloid solution which can be spontaneously dispersed in water to form stable suspension of nano titanium dioxide particles; the nano titanium dioxide particles are crystalline nano titanium dioxide particles.
2. The method for preparing a titanium dioxide material according to claim 1, wherein: the mass fraction of water in the step (2) is five to thirty percent.
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