GB2416164A - A method for synthesising a nanometre-scale titanium dioxide gel - Google Patents

A method for synthesising a nanometre-scale titanium dioxide gel Download PDF

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GB2416164A
GB2416164A GB0415839A GB0415839A GB2416164A GB 2416164 A GB2416164 A GB 2416164A GB 0415839 A GB0415839 A GB 0415839A GB 0415839 A GB0415839 A GB 0415839A GB 2416164 A GB2416164 A GB 2416164A
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acid
transfer process
solution
gel
titanium dioxide
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Wen-Chuan Liu
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052Preparation of gels
    • B01J13/0056Preparation of gels containing inorganic material and water
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052Preparation of gels
    • B01J13/0056Preparation of gels containing inorganic material and water
    • B01J13/006Preparation of gels containing inorganic material and water by precipitation, coagulation, hydrolyse coacervation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0536Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3653Treatment with inorganic compounds
    • C09C1/3661Coating
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Nanotechnology (AREA)
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  • General Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Catalysts (AREA)

Abstract

A method for synthesising a nanometre-scale titanium dioxide gel which comprises the steps of dissolving and diluting a titanium compound, adding ammonia water to produce a precipitate of titanium hydroxide or titanic acid. The precipitate is filtered and the filter cake re-suspended in deionised water and an oxidant or inorganic acid and a modifier and the suspension agitated at an elevated temperature to form a gel, and the pH of the gel is adjusted. The oxidant may be perchloric acid, periodic acid, potassium permanganate, sodium permanganate or nitric acid. The inorganic acid may be perchloric acid, periodic acid, nitric acid, phosphoric acid, hydrochloric acid, sulphuric acid, hydroiodic acid or hydrobromic acid. The modifier may be silicate, polyaluminium chloride, aluminium sulphate or silane. A surfactant may also be added.

Description

TITLE: METHOD FOR SYNTHESIZING HIGH ADSORPTIVE
NANOMETER SCALE TITANIUM DIOXIDE SOLUTION
BACKGROUND OF THE INVENTION
(a) Technical Field ofthe Invention
The present invention relates to method for synthesizing high adsorptive nanometer scale titanium dioxide solution, and particular to a method for synthesizing nanometer scale titanium dioxide solution with high adsorption and which is easily formed as stable film. Namely, a series of chemical process is used to form nanometer scale titanium dioxide sol-gel solution with high adsorption and easily formed as stable films with particles sizes between 2 and 500nm and the content oftitanium dioxide in the solution is between 0.5 and 10 %.
(b) Description ofthe Prior Art
From the 1970s onwards, a large number of research documents disclosed methods for manufacturing semiconductor titanium dioxide. Most ofthe methods use normal chemical components, especially titanium dioxide particles, as raw material. The photochemical l reaction and semiconductor reaction are also discussed. The configuration of crystals and size ofthe particles will affect the efficiency ofthe reactions.
Based on the disclosed documents, to synthesize titanium dioxide photocatalyst, most ofthe prior arts adopts chemical synthesis to make titanium dioxide particles. Although in many cases, the grinding method is used to make titanium dioxides (such as P-25 grinding method used by Degussa Co.). However, this method cannot make titanium dioxide particles with uniform particle size (from 10 to SOO nm) and the crystal configurations cannot matched the required ones. Thereby, it is used in painting, cosmetic, correction fluid, etc. The effect of photo-catalyst cannot be presented.
Although the grinding process is modified, supersonic grinding with supersonic oscillation or chemical grinding with acid liquid is adopted for improving the size and uniformity oftitanium dioxide particles, but the effects ofthese improvements are finite. They cannot greatly improve the configurations of crystals. Thereby, the applications of the products are also confined.
For the chemical synthesis, liquid synthesis is the main method. In the prior art, chemical vapor deposition (CVD) method is adopted to grow titanium dioxide photo-catalyst film, which can provide high stability, high purity photo-catalyst, but manufacturing cost is high and only suitable for some specific products. This prior art cannot be used for mass-production.
Liquid synthesis is classified into two methods, organic solvent method and aqueous method. The aqueous method is a preferred one for making titanium dioxide photo-catalysts.
The organic solvent method uses Ti-alkyloxide: Ti(OR)4 in different solvents so as to form titanium dioxide powder or film depending on the heating process. One ofthese prior arts is disclosed in Japanese Patent No. 4-83537, in that, titanium alkyl- oxide is heated in ethylene glycol. In Japanese Patent No. 7-10037, titanium alkyl-oxide is heated in aminoalcohol so as to get titanium dioxide. Since the titanium alkyl-oxide is expensive and the operation must be performed in high temperature and high pressure.
Thereby, the products by these ways are generally used as industrial chemical catalysts instead of being used in a civil purpose.
The aqueous synthesis are mostly disclosed in Japanese patents or Japanese related documents, such as Japanese Patent No.7-171408, binding agent is added to the titanium tetrachloride and then heated. In Japanese Patent No. 6-293519, under the condition of pH_ 3, titanium tetrachloride solution is directly heated so as to form titanium dioxide sol-gel. The defect of this method is that a large amount of chloride retained so that the sol-gel is unstable and easy to precipitate. In Japanese Patent No. 971418, hydrogen peroxide solution is added to titanium hydroxide, and the pH is 6 to 8 and temperature is lower. In Japanese Patent No. 62-252319, hydrogen peroxide solution is added to titanium hydroxide, and the reaction condition of pH value is from 2 to 6, temperature is low and reaction time is longer. The particle size ofthe titanium dioxide sol-gel generated by these way is about 10 nanometers.
Since the particles are mainly non-crystal, it is suitable for surface treatment, but it is not an effective photo-catalyst. In Japanese Patent No. 7-28614, pertitanic acid is heated and in Japanese Patent No. 285993, hydrogen peroxide solution is added to titanium hydroxide and then reaction temperature is increased so as to form titanium dioxide sol-gel. The products have photo-catalytic effect. Due to the property of hydrogen peroxide, the concentration ofthe titanium dioxide sol-gel is confined to be below 2%.
Therefore, it cannot be widely used.
In Taiwan Patent No. 135895, titanium tetrachloride solution is added with organic acid. Then the solution is heated at temperature above 70 C so as to form anatase titanium dioxide. The titanium dioxide sol-gel produced by this way is the right configuration and particle size, but the content of chloride is high (above 10 grams / liter). Thus, the stability ofthe product is not preferred.
In Taiwan Patent No.349981, the titanium tetrachloride reacts with ammonia water with a pH value of 2 to 6. Then the precipitate (titanium hydroxide or titanic acid) is filtered and rinsed. Hydrogen peroxide is added into the solution in low temperature (5 to 8 C). The solution is agitated for a s longer time so as to disperse non-crystal titanium dioxide which is unrelated to the present invention. In Taiwan Patent No. 393342, the titanium sulfate is heated to form titanium dioxide and then mono-proton acid (such as nitric acid, etc.) is added to the titanium dioxide for removing residue sulfate and solving titanium dioxide to reduce the particle size of the titanium dioxide. This prior art is also unrelated to the present invention. Taiwan Patent No. 443992 discloses a method for forming titanium dioxide film instead of sol-gel.
Another method for synthesizing the solution comprises the steps of dissolving, diluting, neutralizing (above steps are used in the prior art) , and l O cleaning, form-transferring and formation the titanium compound in a predetermined acid liquid to acquired nanometer scale titanium dioxide photo-catalyst sol-gel. This prior art method is a skilled process which is stable and suitable for mass-production, but this process is only used in the titanium dioxide sol-gel which is not suitable for the succeeding steps and do not match to the processed objects.
As mentioned above, it is found that all the prior arts are aimed at titanium dioxide sol-gel, but the succeeding process and the object to be treated are not taken into consideration. The titanium dioxide sol-gel has no preferred adsorption and is not stable for a long time. Therefore, the application ofthe titanium dioxide sol-gel is confined.
SUMMARY OF THE INVENTION
Accordingly, the primary object ofthe present invention is to provide a method for synthesizing high adsorptive nanometer scale titanium dioxide, wherein a series of chemical process is used to form nanometer scale titanium dioxide sol-gel solution. It is an adsorptive material with a particle size between 2 and 500nm and the content oftitanium dioxide is between 0.5 and %. It can easily form a suitable film.
To achieve the above objects, the present invention provides a method for synthesizing high adsorptive nanometer scale titanium dioxide, wherein titanium tetrachloride or titanium sulfate is dissolved and diluted in acid liquid and then ammonia water is added to neutralize the solution with pH between 7 and 9 so as to generate titanium hydroxide. After washing or filtering, at the form-transfer process; clean titanic acid is agitated with de-ionized water and uniformly mixed; then predetermined amount of oxidant or inorganic acid and modifier is added. At the formation process; the form-transferred solution being performed with formation process in a predetermined temperature and time so as to get a sol-gel. The titanium dioxide sol-gel can be applied to a surface of an object to be treated so as to form the film with preferred adsorption.
The foregoing object and summary provide only a brief introduction to the present invention. To fully appreciate these and other objects ofthe present invention as well as the invention itself, all of which will become apparent to those skilled in the art, the following detailed description of the invention and the claims should be read in conjunction with the accompanying drawings. Throughout the specification and drawings identical reference numerals refer to identical or similar parts.
Many other advantages and features ofthe present invention will become manifest to those versed in the art upon making reference to the detailed description and the accompanying sheets of drawings in which a preferred structural embodiment incorporating the principles ofthe present invention is shown by way of illustrative example.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 shows the flow chart ofthe present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following descriptions are of exemplary embodiments only, and are not intended to limit the scope, applicability or configuration of the invention in any way. Rather, the following description provides a convenient illustration for implementing exemplary embodiments of the invention.
Various changes to the described embodiments may be made in the function and arrangement ofthe elements described without departing from the scope ofthe invention as set forth in the appended claims.
In order that those skilled in this art can further understand the present invention, a description will be present in the following in detail. However, these descriptions and the appended drawings are only used to show those skills in the art to understand the objects, features, and characteristics ofthe present invention, but not to be used to confine the scope and spirit ofthe present invention defined in the appended claims.
The present invention provides a method for synthesizing high adsorptive nanometer scale titanium dioxide solution. The method comprises the prior art with steps of dissolving, diluting, neutralizing, and cleaning titanic compound in predetermined acid liquid to acquire titanium hydroxide or titanic acid. The titanium hydroxide is transferred into nanometer scale crystal titanium dioxide sol-gel with functions of photo- catalyst and self-cleaning. The method further comprises the following steps: A form-transfer process in predetermined condition is performed. Clean titanic acid is agitated with de-ionized water and thus the titanic acid is uniformly mixed. Predetermined amount of oxidants or inorganic acids (or organic acid), and modifiers are added.
Then a formation process is performed for the form-transferred solution in a predetermined temperature and time so as to get titanium dioxide solgel.
The pH value ofthe sol-gel is adjusted and the titanium dioxide sol-gel is filtered from the solution. Finally, the filtered sol-gel is packaged.
l O With reference to Fig. l, the method for synthesizing high adsorptive nanometer scale titanium dioxide solution of the present invention is mainly for improving the bad adsorption and film property as that are manufactured from prior art. The novel process ofthe present invention is that the titanium dioxide sol-gel is further performed with the process of form transfer and formation so as to acquire titanium dioxide sol-gel with functions of photo-catalyst and self-cleaning.
In the form transfer process, the cleaned filter cake lO oftitanium hydroxide l (or called as titanic acid) is added in de-ionized water 11. The solution is agitated through 12 minutes. Then oxidant 2 or inorganic acid 21 is added to the solution as required. Then modifier 3 and required surfactant 4 are added. In the present invention, the oxidant 2 is selected from at least one of perchloric acid, periodide acid, potassium permanganate, sodium permanganate, and nitric acid; and 1 to 200 grams / liters oxidant is added.
The inorganic acid 21 is selected from at least one of perchloric acid, periodide acid, nitric acid, phosphoric acid, hydrochloric acid, sulfuric acid, and hydrogen iodide, hydrobromic acid; per liter solution is added with 1 to 120 grams inorganic acid. The organic acid is selected from one of oxalic acid, citric acid, picric acid, formic acid, acetic acid, benzoic acid, salicylic acid, and derivatives of ammonium compounds; and the added inorganic acid in the form transfer-process is between 0.1 gram / liter to 150 grams / liter. The modifier 3 is selected from one of silicate, Poly-aluminium chloride(PAC), aluminium sulfate, and silane depending on a final product required; the amount of modifier used in form-transfer process is between 0.0575 milliliter / liter. The surfactant 4 used in form-transfer process is selected from one of l S polyvinyl alcohol (PVA); polypropylene alcohol (PPA); and mixture of polyvinyl alcohol (PVA)/ polypropylene alcohol (PPG); poly- alcohols selecting from adding Polyethylene glycol, Polypropylene glycol and butadiene Polypropylene; and poly-ethers selecting from Polyoxyethylene phenol ether / Polyoxypropylene alkyl phenol ether / Polyoxypropylene phenol ether / Polyoxypropylene alkyl phenol ether, and Polyoxyethylene Polyoxypropylene ether; and a molecular weight of the surfactant used in the form-transfer process is between 200 - 7000. The amount of interface activator used in form-transfer process is between 1 0 - 15000 ppm and the agitating speed is between 30 - 300 rpm; the time for form-transfer process is 10 to 120 minutes; and the temperature in form-transfer process is retained at 10to95 C. One or both ofthe oxidant 2 and the acid 21 can be added to the de-ionized water solution, which is determined by the requirement of final product. If the titanium dioxide sol-gel solution is directly used to spray a surface, the oxidant 2 is a preferred selection. If the final sol-gel is used to form film or to final finish work, or requires higher density, inorganic acid 21 is a preferred selection, or both the oxidant or the inorganic acid 21 are used. The selection of inorganic acid is based on the object to be used and the environment.
The modifier 3 is determined by the objects to be treated, for example, for natural materials, such as wood, paper, fibers, etc., the silicate, poly-aluminium chloride(PAC), and aluminium sulfate are preferred. For glass, metal, stone, ceramic, etc., silicate is preferred. For manmade fibers, polymers, silicate and silane, are preferred.
The titanic acid added with modifier 3 and oxidant 2 or inorganic acid 21 is form-transferred in a set oftemperature and time. In the present invention, the agitating speed is between 30 - 300 rpm; the time for formtransfer process is 10 to 120 minutes; and the temperature in formtransfer process is retained at 10 to 95 C. The solution after formtransfer process is executed with the formation process. The agitating speed in formation process is from 30 to 300 rpm with a temperature between 50 and 95 C through a time period of 4 to 72 hours which are determined by a desired product; The titanium dioxide sol-gel 5 after formation is performed with the steps of pH adjusting, filtering, and package; wherein the pH adjuslent is performed according to requirements of the product.
In the following, a plurality of embodiments about the method ofthe present invention will be illustrated so that those skills in the art can understand the present invention.
FIRST EMBODIMENT
In the first embodiment of the present invention, the method for synthesizing high adsorptive nanometer scale titanium dioxide solution is performed by the following processes. Ten liters de-ionized water is added to a reaction tank with a volume of 20 liters. The agitating speed is set at 300 rpm.
The reaction tank is retained in temperature of 5 to l0 C by ice-water bath.
A predetermined amount, 500 grams, oftitanium tetrachloride (with a ratio of 98%) is added to the water with a speed of 4 ml / min by using a dosing pump.
When all the titanium tetrachloride is added and agitated through 2 hours until the liquid is clear and become transparent, ammonia water with a concentration of 20 % is added with an addition speed of 10 ml / min and an agitation speed of 600 rpm. Variation of pH value is monitored. When the pH value is attained to 4.0, the addition speed is changed to 2 - 4 ml / min until the pH value is achieved to 7.5 to 8.0. The above solution is filtered with a vacuum filter. Then a filter cake (containing titanium hydroxide) from the solution is added to a clean 200 liter tank. The tank has been filled with 100 liters running water or soft water. The agitation speed is set at 600 rpm and the agitation time period is 2 hours until the filter cakes are Uniformly mixed.
Then it is filtered. The process of cleaning and filtering are repeated three times. Then the filter cake is transferred to a form-transfer and formation tank.
liters de-ionized water is added to the tank. The agitation speed is retained at 300 rpm. The filter cake is added and then the solution is agitated through one hour so that they are mixed uniformly. Then 50 ml of perchloric acid (HC104) is added to the solution. The solution is agitated through 80 min. The temperature of solution is increased to 80 to 90 C. The solution is agitated through 6 hours. The temperature of the solution is decreased and pH is adjusted. Then the solution is packaged as product. In the present invention, the acquired titanium dioxide sol-gel is colorless or yellow transparent solution with a pH value of about 5 to 9. The content oftitanium dioxide is about 1% and the particle size is about 5 to 50 nm, which is presented as needle-like or sheet-like crystal. The present invention can be directly used in spray treatment or is processed as film so as to have the function of self-cleaning.
If the solution of the present invention is radiated by ultra-violet light, it has the function of sterilization. The product is performed with spraying treatment, and then dried at room temperature to become a thin film. Then an adhesion test by using 3M tape is applied to the film. As a result, it appear that no film falls off, but in the prior art, for the film of titanium dioxide sol-gel without adding silicic acid, when the film is experienced with spraying treatment, the film will fall offin the test. Hence, the present invention is better then the
prior art.
SECOND EMBODIMENT
The process is identical to the first embodiment except that in the formtransfer process, 100 milliliter ofthe poly aluminium chloride (10%) is used to replace silicic acid. Operation conditions are same as the first embodiment. The acquired titanium dioxide sol-gel is yellow transparent solution with a pH value between 7 and 9. The content of titanium dioxide is 1%. The particle size is about 5 to 30 rim with needle - like or sheetlike crystals. The product can be directly used in spray treatment and then is processed as film so as to have the function of self-cleaning. If the solution of the present invention is radiated by ultra-violet light, it has the function of sterilization. The product is performed with spraying treatment, and then dried at room temperature to become a thin film. Then the adhesion test by using 3M tape is applied to the film. As a result, it appears that no product falls off, but for the film oftitanium dioxide sol-gel without adding silicic acid, when the film undergoes spraying treatment, the film will fall offin the test.
THIRD EMBODIMENT
The process is the same as the first embodiment, but in the final formation process, the agitation time is prolonged to 48 hours from the original six hours. The acquired titanium dioxide sol-gel is transparent or yellow transparent solution with a pH value between 4 and 9. The content of titanium dioxide is 1 %. The particle size is about 20 to 100 rim with needle - like or sheet - like crystals. The product is directly performed with spraying treatment, and then dried at room temperature to become a thin film.
As a result, it appears that an object coated with the film can be cleaned by water easily. Because there is no function of photo-catalyst in the film, organic material will not be destroyed. Thereby, the film has preferred adhesive ability so that it can be widely used in furniture or daily-used articles.
FOURTH EMBODIMENT
The process is identical to the third embodiment except that in the formtransfer process, 10 milliliters of silane is used to replace silicic acid.
Operation conditions are same as the first embodiment. The acquired titanium dioxide sol-gel is transparent or yellow transparent solution with a pH value between 7 and 9. The content of titanium dioxide is I %. The particle size is about 5 to 30 rim with needle-like or sheet-like crystals. The product can be directly used in spray treatment and then is processed as films by heating on manmade fiber / high molecular polymer products so as to have the function of self-cleaning. It can be washed easily. The product is performed with spraying treatment, and then dried at room temperature on a plastic article to form as a thin film. Then an adhesion test is performed by adhering 3M tape on the articles. No film falls off, but for the prior art film oftitanium dioxide sol-gel without silicic acid, when the film undergoes spraying treatment, the film will fall off in the test.
FIFTH EMBODIMENT
The process is identical to the third embodiment except that the product is sprayed on ceramics coated with glaze (not sintered). Then they are sintered.
As a result, the surface ofthe ceramics is harder, pollution-proofed and easy to be washed.
SIXTH EMBODIMENT
The process is same as the fourth embodiment, but in the form-transfer process, the amount ofthe filter cake and additives are increased to ten times than the original one. The product is dried In vacuum environment (with a temperature less than 70 C) so as to form as powder. The powder can be used in the brightness surface treatment of various materials for increasing the wear-resistance of the material. Furthermore, the product is difficult to be polluted and is easy to be washed.
Advantages ofthe present invention are that the product ofthe present invention is difficult to be polluted and can be washed easily. Moreover, the present invention has preferred wear-resistance.
It will be understood that each ofthe elements described above, or two or more together may also find a useful application in other types of methods differing from the type described above.
While certain novel features ofthis invention have been shown and described and are pointed out in the annexed claim, it is not intended to be limited to the details above, since it will be understood that various omissions, modifications, substitutions and changes in the forms and details ofthe device illustrated and in its operation can be made by those skilled in the art without departing in any way from the spirit ofthe present invention.

Claims (16)

  1. I CLAIM: 1. A method for synthesizing high adsorptive nanometer scale
    titanium dioxide solution comprising the steps of dissolving, diluting, neutralizing, and cleaning titanic compound in predetermined acid liquid to acquire clean powder oftitanium hydroxide or titanic acid; after the powder precipitate in the acid liquid, the powder being synthesized into nanometer scale crystal titanium dioxide sol-gel with functions of photocatalyst and self-cleaning; the method further comprising the steps of: executing a form-transfer process in predetermined condition; clean titanic acid being agitated with de-ionized water and thus the titanic acid being uniformly mixed with de-ionized water; and then predetermined oxidants or inorganic acids, and modifiers being added to the de-ionized water solution; executing a formation process; the form-transferred solution being performed with formation process in a predetermined temperature and time so as to get a sol-gel; adjusting the pH ofthe solgel; filtering the sol-gel from the solution; and packaging the filtered sol-gel.
  2. 2. The method as claimed in claim 1, wherein the titanic compound is one oftitanium hydroxide and titanic acid.
  3. 3. The method as claimed in claim 1, further comprising the step of mixing washed filtered cakes into the de-ionized water and then agitating the de-ionized water solution; and then adding the predetermined oxidant or inorganic acid and modifier / interface activator to the mixing solution.
  4. 4. The method as claimed in claim 1, wherein the oxidant is selected from at least one of perchloric acid, periodide acid, potassium permanganate, sodium permanganate, and nitric acid; and 1 to 200 grams / liters oxidant is added.
  5. 5. The method as claimed in claim 2, wherein the oxidant is selected from at least one of perchloric acid, periodide acid, potassium permanganate, sodium permanganate, and nitric acid; and 1 to 200 grams / liters oxidant is added.
  6. 6. The method as claimed in claim 1, wherein the inorganic acid is selected from at least one of perchloric acid, periodide acid, nitric acid, phosphoric acid, hydrochloric acid, sulfuric acid, and hydrogen iodide, hydrobromic acid; I to 120 grams inorganic acid is added to per liter solution.
  7. 7. The method as claimed in claim 2, wherein the inorganic acid is selected from at least one of perchloric acid, periodide acid, nitric acid, phosphoric acid, hydrochloric acid, sulfuric acid, and hydrogen iodide, hydrobromic acid; 1 to 120 grams inorganic acid is added to per liter solution.
  8. 8. The method as claimed in claim 1, wherein the inorganic acid is selected from one of oxalic acid, citric acid, picric acid, formic acid, acetic acid, benzoic acid, salicylic acid, and derivatives of ammonium compounds; and the added inorganic acid in the form transfer-process is between 0.1 gram / liter to 150 grams / liter.
  9. 9. The method as claimed in claim 2, wherein the inorganic acid is selected from one of oxalic acid, citric acid, picric acid, formic acid, acetic acid, benzoic acid, salicylic acid, and derivatives of ammonium compounds; and the added inorganic acid in the form transfer-process is between 0.1 gram / liter to 150 grams / liter.
  10. 10. The method as claimed in claim 1, wherein the modifier is selected from one of silicate, Poly-aluminum chloride(PAC), aluminum sulfate, silane depending on the final product required; the amount of modifier used in form-transfer process is between 0.0575 milliliter / liter.
  11. 11. The method as claimed in claim 2, wherein the modifier is selected from one of silicate, Poly-aluminium chloride(PAC), aluminium sulfate, silane depending on the final product required; the amount of modifier used in form-transfer process is between 0.0575 milliliter / liter.
  12. 12. The method as claimed in claim 1, wherein the surfactants used in form-transfer process is selected from one of polyvinyl alcohol (PVA); polypropylene alcohol (PPA); and mixture of polyvinyl alcohol (PVA)/ polypropylene alcohol (PPA); poly-alcohols selecting from adding Polyethylene glycol, Polypropylene glycol and butadiene Polypropylene; and ploy-ethers selecting from Polyoxyethylene phenol ether / Polyoxypropylene alkyl phenol ether / Polyoxypropylene phenol ether / Polyoxypropylene alkyl phenol ether, and Polyoxyethylene Polyoxypropylene ether; and a molecular weight ofthe surfactants used in the form-transfer process is between 200 - 7000.
  13. 13. The method as claimed in claim 2, wherein the surfactants used in form-transfer process is selected from one of polyvinyl alcohol (PPA); polypropylene alcohol (PPA); and mixture of polyvinyl alcohol (PVA)/ polypropylene alcohol (PPA); poly-alcohols selecting from adding Polyethylene glycol, Polypropylene glycol and butadiene Polypropylene; and ploy-ethers selecting from Polyoxyethylene phenol ether / Polyoxypropylene alkyl phenol ether / Polyoxpropylene phenol ether / Polyoxypropylene alkyl phenol ether, and Polyyoxyethylene Polyoxypropylene ether; and a molecular weight ofthe surfactants used in the form-transfer process is between 200 - 7000.
  14. 14. The method as claimed in claim 1, wherein the amount of surfactants used in form-transfer process is between 10 - 15000 ppm and the agitating speed is between 30 - 300 rpm; the time for form-transfer process is 10 to 120 minutes; and the temperature in form-transfer process is retained at 10 to 95 C.
  15. 15. The method as claimed in claim 8, wherein the amount of surfactants used in form-transfer process is between 10 - 15000 ppm and the agitating speed is between 30 - 300 rpm; the time for form-transfer process is lO to 120 minutes; and the temperature in form-transfer process is retained at 10 to 95 C.
  16. 16. The method as claimed in claim 1, wherein the solution after form- transfer process is executed with the formation process in an original tank or a predetermined formation tank; agitating speed in formation process is from 30 to 300 rpm with a temperature between 50 and 95 C through a time period of 4 to 72 hours which are determined by a desired product; the sol-gel is performed with the process of pH adjusting, filtering, and package; wherein the pH adjustment is performed according to requirements ofthe product.
GB0415839A 2004-07-15 2004-07-15 A method for synthesising a nanometre-scale titanium dioxide gel Withdrawn GB2416164A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN101844805A (en) * 2010-06-08 2010-09-29 上海工程技术大学 Method for preparing aqueous high-dispersion nano titanium dioxide
CN107935138A (en) * 2017-11-22 2018-04-20 广东桑海环保有限公司 A kind of ionic control agent and its preparation method and application

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115090076B (en) * 2022-07-05 2023-07-21 王西峰 Quartz glass fiber loaded titanium dioxide photocatalyst filler and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
JPS63123815A (en) * 1986-11-10 1988-05-27 Ishihara Sangyo Kaisha Ltd Neutral titania sol and production thereof
US5403513A (en) * 1987-10-07 1995-04-04 Catalyst & Chemical Industries, Co., Ltd. Titanium oxide sol and process for preparation thereof

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Publication number Priority date Publication date Assignee Title
JPS63123815A (en) * 1986-11-10 1988-05-27 Ishihara Sangyo Kaisha Ltd Neutral titania sol and production thereof
US5403513A (en) * 1987-10-07 1995-04-04 Catalyst & Chemical Industries, Co., Ltd. Titanium oxide sol and process for preparation thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844805A (en) * 2010-06-08 2010-09-29 上海工程技术大学 Method for preparing aqueous high-dispersion nano titanium dioxide
CN107935138A (en) * 2017-11-22 2018-04-20 广东桑海环保有限公司 A kind of ionic control agent and its preparation method and application

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