WO2022007764A1 - Méthode de préparation de dioxyde de titane et méthode d'amélioration de la dispersibilité du dioxyde de titane - Google Patents

Méthode de préparation de dioxyde de titane et méthode d'amélioration de la dispersibilité du dioxyde de titane Download PDF

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WO2022007764A1
WO2022007764A1 PCT/CN2021/104594 CN2021104594W WO2022007764A1 WO 2022007764 A1 WO2022007764 A1 WO 2022007764A1 CN 2021104594 W CN2021104594 W CN 2021104594W WO 2022007764 A1 WO2022007764 A1 WO 2022007764A1
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titanium dioxide
dispersibility
titanium
improving
nano
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PCT/CN2021/104594
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梁先华
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宁波极微纳新材料科技有限公司
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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
    • 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

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  • the present application relates to a method for preparing titanium dioxide and a method for improving the dispersibility of titanium dioxide.
  • Nano-titanium dioxide refers to titanium dioxide with a particle size of less than 100 nanometers. It has special effects such as small particle size, high specific surface area, excellent photocatalytic activity, stable chemical and thermal properties, and super affinity. Self-cleaning materials, sunscreen skin care products and other fields have irreplaceable application advantages. For example, 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 liquid phase synthesis method has the advantages of easy control of the reaction, simple equipment, and low 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, etc.
  • the process route of the precipitation method means that at a certain temperature, by controlling the pH value of the solution, the titanium source is hydrolyzed in water to form insoluble hydrated titanic acid precipitation, and then the titanium dioxide powder is obtained by filtering, washing, drying, calcining and other steps. body.
  • the calcination temperature is usually greater than 500 degrees Celsius. The high calcination temperature also increases the equipment investment and energy consumption in the synthesis process.
  • reducing the calcination temperature in the precipitation method is a key step to improve the synthesis of titania materials by the precipitation method, which is of great significance for improving product performance and reducing costs.
  • Nanoparticles with ultra-small particle size can exhibit more excellent properties in energy, environment, and catalysis.
  • titanium dioxide materials with a particle size of less than 100 nanometers have special effects such as small particle size, high specific surface area, excellent photocatalytic activity, stable chemical and thermal properties, and super affinity, which are used in air treatment, sterilization and self-cleaning. Materials, sunscreen skin care products and other fields have irreplaceable application advantages.
  • nano-titania particle dispersion have important effects on the reaction process and the final product.
  • product performance largely depends on the dispersion degree of titanium dioxide powder in liquid medium.
  • the application effect is also better.
  • nano-TiO2 particles are small in size, have a large number of defects on the surface, large surface activity, and are in a thermodynamically unstable state.
  • the nanoparticles dispersed in the liquid medium are easy to coagulate, agglomerate, and coagulate, and cannot form a stable dispersion.
  • Preventing the agglomeration of nano-titanium dioxide particles and obtaining monodisperse titanium dioxide nanoparticles can greatly improve the performance of titanium dioxide nanomaterials in the fields of optics, electricity, and catalysis.
  • the physical dispersion method mainly uses external forces to disperse the nanoparticles, including mechanical stirring dispersion, ultrasonic dispersion and high-energy treatment dispersion.
  • the disadvantage of the physical dispersion method is that if the external force stops, the particles will re-aggregate.
  • the chemical dispersion method is to use surface chemical methods to add surface treatment agents for dispersion.
  • the preparation of water-phase dispersed nanoparticles is usually achieved by the induction and restraint of water-soluble surfactants or polymers, but the surface of the particles is covered with modified molecules such as organics.
  • modified molecules such as organics.
  • the contribution of dispersibility control to improving material properties is reduced, such as the preparation of water-soluble titanium dioxide nanoparticles by the reaction of titanium alkoxides and alkylamines, but the presence of such alkaline reagents passivates the surface activity of the product to make it photocatalytic
  • different application systems may also have adverse adverse effects with the surface-modified molecules, reducing the application performance of the final product.
  • the use of polyethylene glycol as a stabilizer makes the dispersibility of titanium dioxide nanoparticles somewhat improved.
  • the titanium dioxide dispersion product obtained by the above method is still a liquid suspension, the particles cannot be completely monodispersed and the particle size is uneven, and a stable colloidal dispersion cannot be formed, resulting in high transportation costs and practical application.
  • the present invention provides a technical method for preparing low-temperature crystallized titanium dioxide, so as to improve the precipitation synthesis method of nano-titanium dioxide and promote the properties and application fields of titanium dioxide nanomaterials.
  • Another object of the present invention is to provide a technical method for greatly improving the dispersibility of nano-titanium dioxide, so as to promote the application field and use effect of nano-titanium dioxide materials.
  • the present invention adopts the following technical solutions:
  • a method for preparing low-temperature crystallized titanium dioxide comprising the following steps:
  • the titanium compound is hydrolyzed, separated, purified and dried to obtain hydrated titanic acid
  • the titanium compound is selected from one or a combination of titanium sulfate, titanium oxysulfate, titanium tetrachloride, titanium isopropoxide, and tetrabutyl titanate.
  • the hydrolysis process is to directly react the titanium compound with water; or, the hydrolysis process is to react the titanium compound with an alkaline aqueous solution.
  • the passing hydrogen chloride gas also contains water vapor.
  • the pressure of the constant pressure reaction is 0.5 atmospheres to 20 atmospheres; the preferred pressure is 1 atmosphere to 10 atmospheres.
  • the time of the constant pressure reaction is 3 hours to 24 hours.
  • the crystal phase of the crystalline nano-titania material is rutile phase or anatase phase or a composite phase of rutile phase and anatase phase.
  • the crystalline nano-titania material can be spontaneously dispersed in pure water without additives or dispersants to form a stable dispersion; the dispersion is mainly colloidal dispersion.
  • the crystalline nano-titanium dioxide material is nano-scale titanium dioxide particles with a particle size of less than 100 nanometers or nano-scale titanium dioxide particle agglomerates with a particle size of less than 100 nanometers; the surface of the crystalline nano-titanium dioxide material is Acidic.
  • a method for improving the dispersibility of titanium dioxide comprising the following steps:
  • the precursor solid titanium dioxide A is thermally treated in a hydrogen chloride atmosphere to obtain a dispersed titanium dioxide B product.
  • a method and product for improving the dispersibility of titanium dioxide comprising the following steps:
  • the precursor solid titanium dioxide A is placed in the container;
  • the container in which the precursor solid titanium dioxide A is placed is filled with hydrogen chloride gas and subjected to low temperature heating treatment to obtain a dispersible titanium dioxide B product.
  • the dispersibility of the dispersible titanium dioxide B product in water is increased by more than ten times.
  • the dispersion stability of the dispersible titanium dioxide B product in water is improved by more than ten times.
  • the transparency of the dispersible titanium dioxide B product after being dispersed in water is increased by more than ten times.
  • the dispersible titanium dioxide B product can spontaneously disperse in pure water without additives or dispersants to form a stable dispersion; the dispersion is mainly colloidal dispersion.
  • the dispersible titanium dioxide B product is nanoscale titanium dioxide particles with a particle size of less than 100 nanometers or nanoscale titanium dioxide particle agglomerates with a particle size of less than 100 nanometers; the surface of the dispersible titanium dioxide B product is Acidic.
  • the dispersible titanium dioxide B product is crystalline nano-titanium dioxide; the crystal phase of the crystalline nano-titanium dioxide is one or more of anatase phase, rutile phase, and brookite phase The combination.
  • the precursor solid titanium dioxide A is nanoscale titanium dioxide particles with a particle size of less than 100 nanometers or nanoscale titanium dioxide particle agglomerates with a particle size of less than 100 nanometers.
  • the precursor solid titanium dioxide A is nanoscale titanium dioxide particles with a particle size of less than 50 nanometers or nanoscale titanium dioxide particle agglomerates with a particle size of less than 50 nanometers.
  • the precursor solid titanium dioxide A is crystalline titanium dioxide particles or amorphous titanium dioxide particles.
  • the precursor solid titanium dioxide A further includes one or a combination of titanium hydroxide, titanium hydroxide hydrate, titanic acid, and titanic acid hydrate.
  • the hydrogen chloride atmosphere also contains water vapor; the pressure of the water vapor is 0.1 atm to 10 atm.
  • the pressure of the hydrogen chloride gas in the hydrogen chloride atmosphere is 0.5 atm to 20 atm.
  • the pressure of the hydrogen chloride gas in the hydrogen chloride atmosphere is 1 atmosphere to 10 atmospheres.
  • the pressure of the hydrogen chloride gas in the hydrogen chloride atmosphere can be constant or changed.
  • the hydrogen chloride atmosphere is provided in a continuous manner or an intermittent manner.
  • the source of the hydrogen chloride atmosphere can be provided by the inside of the reaction system or provided by external input.
  • the temperature of the heat treatment is 80 degrees Celsius to 300 degrees Celsius; the preferred heat treatment temperature is 100 degrees Celsius to 200 degrees Celsius.
  • the time of the heat treatment is 2 hours to 48 hours.
  • the hydrogen chloride gas in the hydrogen chloride atmosphere fluctuates within a predetermined pressure range; the hydrogen chloride atmosphere is provided in a continuous manner; the hydrogen chloride atmosphere is provided by an external input.
  • the method for preparing low-temperature crystalline titanium dioxide greatly reduces the calcination temperature in the nano-titanium dioxide precipitation synthesis method, and reduces the calcination temperature from 500 degrees Celsius to a minimum of 100 degrees Celsius, saving energy consumption and equipment investment.
  • the nano-titanium dioxide material obtained by the method for preparing low-temperature crystalline titanium dioxide has a great improvement in specific surface area, dispersibility and catalytic performance.
  • the method for improving the dispersibility of titanium dioxide does not use any surface organic additives, which makes the application field of the nano-titanium dioxide dispersion liquid universal, and increases the application field and use effect of the dispersion liquid.
  • the method for improving the dispersibility of titanium dioxide has low processing temperature, simple operation steps and low price, which is favorable for large-scale industrialization and application.
  • FIG. 1 is a transmission electron microscope image observed after the titanium dioxide water dispersion droplets obtained in Example 1 are coated on a copper mesh and dried.
  • Example 2 is an X-ray diffraction pattern of the titanium dioxide product prepared in Example 1, and the main crystal phase is anatase phase.
  • FIG. 3 is a colloidal water dispersion formed by mixing the titanium dioxide material obtained in Example 1 with water.
  • Fig. 4 is the photocatalytic degradation curve of rhodamine B of the nano-titania product obtained in Example 1 and P25.
  • Fig. 5 is that the mass fraction obtained after adding water to the nano-titania product obtained in Example 4 is an aqueous dispersion of 5/1000, which has a relatively stable dispersion state;
  • Figure 6 is an optical image of the precursor titanium hydroxide suspension with a mass fraction of 5/1000 standing for 2 hours, with obvious delamination phenomenon, and the suspension is unstable;
  • Fig. 7 is the SEM image obtained by drip-coating the product obtained in Example 4 on a silicon wafer after being dispersed in water, and observed after drying;
  • Fig. 8 is the scanning electron microscope image obtained after the precursor titanium hydroxide is dispersed in water and then drop-coated on the silicon wafer and observed after drying;
  • FIG. 9 is a scanning electron microscope image of the product obtained in Comparative Example 3, after being dispersed in water and then drop-coated on a silicon wafer, and observed after drying.
  • Fig. 2 is the X-ray diffraction pattern of the titanium dioxide product prepared in this example, it can be seen from Fig. 2 that the main crystal phase of the nano-titanium dioxide obtained in this example is anatase phase, which has good crystallinity, and further illustrates the present invention
  • the calcination temperature in the nano-titanium dioxide precipitation synthesis method can be greatly reduced, and the calcination temperature is reduced from 500 degrees Celsius to 160 degrees Celsius.
  • the nano-titanium dioxide product obtained in this example is added to water to obtain a nano-titanium dioxide dispersion with a mass fraction of 5/1000.
  • the dispersion has good monodispersity and can form stable in an aqueous solution.
  • the colloidal dispersion of the nanoparticle is stable in suspension, does not agglomerate and is not easy to settle, and the solution is placed for more than 6 months without stratification.
  • the nano-titania material obtained in this example has good photocatalytic activity, and the catalytic efficiency is 9 times that of commercial P25 material.
  • 1 gram of Degussa) sample was dispersed in 100 ml of Rhodamine B solution with a concentration of 2.0 ⁇ 10-5 mol per liter, and was placed in a dark place with magnetic stirring for 30 minutes to achieve temperature equilibrium and adsorption equilibrium. Then turn on the simulated sunlight lamp, stir, take out 3 ml of samples at regular intervals, separate the particles by centrifugation, measure the absorbance of the solution at 550 nm with a UV-Vis spectrometer, and calculate the remaining concentration of Rhodamine B.
  • the advantages of the present invention are: (1) the technical method greatly reduces the calcination temperature in the nano-titanium dioxide precipitation synthesis method, and reduces the calcination temperature from 500 degrees Celsius to 160 degrees Celsius, saving energy consumption and equipment investment. (2) The nano-titanium dioxide material obtained by this technical method is greatly improved in terms of specific surface area, dispersibility and catalytic performance.
  • the particle size of the product titanium dioxide nanoparticles is 10 nanometers to 20 nanometers. Nanometer, and further illustrate that the nanometer titanium dioxide obtained in this example has a small particle size and good monodispersity.
  • the X-ray diffraction pattern confirms that the main crystal phase of the titanium dioxide product obtained in this implementation is anatase phase, which has good crystallinity, and further shows that the present invention can greatly reduce the calcination temperature in the nano-titanium dioxide precipitation synthesis method. Reduced from 500 degrees Celsius to 120 degrees Celsius.
  • the nano-titanium dioxide product obtained in this example is added to water to obtain a nano-titanium dioxide dispersion with a mass fraction of 5/1000.
  • the dispersion has good monodispersity and can form a stable colloidal dispersion in an aqueous solution. Nanoparticles are stably suspended, do not agglomerate and are not easy to settle, and the solution has not been delaminated for 10 months.
  • the nano-titanium dioxide material obtained in this example has good photocatalytic activity, and the catalytic efficiency is 6 times that of commercial P25 material.
  • the specific comparison method is to weigh the product obtained in this example and the P25 (Degusa) sample 1 gram respectively. Disperse in 100 ml of Rhodamine B solution with a concentration of 2.0 ⁇ 10-5 moles per liter, and place it in a dark place with magnetic stirring for 30 minutes to achieve temperature equilibrium and adsorption equilibrium.
  • the X-ray diffraction pattern confirms that the main crystal phase of the titanium dioxide product obtained in this implementation is rutile phase, which has good crystallinity, and further shows that the present invention can greatly reduce the calcination temperature in the nano-titanium dioxide precipitation synthesis method, and the calcination temperature is increased from 500 Celsius decreased to 200 degrees Celsius.
  • the nano-titanium dioxide product obtained in this example is added to water to obtain a nano-titanium dioxide dispersion with a mass fraction of one thousandth.
  • the dispersion has good monodispersity and can form a stable colloidal dispersion in an aqueous solution. Nanoparticles are stably suspended, do not agglomerate and are not easy to settle, and the solution does not delaminate after being placed for 1 month.
  • the nano-titania material obtained in this example has good photocatalytic activity, and the catalytic efficiency is twice that of commercial P25 material.
  • the specific comparison method is to weigh the product obtained in this example and the P25 (Degussa) sample 1 gram respectively. Disperse in 100 ml of Rhodamine B solution with a concentration of 2.0 ⁇ 10-5 moles per liter, and place it in a dark place with magnetic stirring for 30 minutes to achieve temperature equilibrium and adsorption equilibrium. Then turn on the simulated sunlight lamp, stir, take out 3 ml of samples at regular intervals, separate the particles by centrifugation, measure the absorbance of the solution at 550 nm with a UV-Vis spectrometer, and calculate the remaining concentration of Rhodamine B. Comparative Example 1
  • titanium hydroxide (Guangdong Wengjiang Chemical Reagent Co., Ltd., CAS No.: 20338-08-3, purity ⁇ 99%) powder was weighed and placed in a pressure-resistant anti-corrosion tube. Then, heat the pressure-resistant anti-corrosion pipe to 120 degrees Celsius, keep the pressure of the hydrogen chloride injection port in the pipe about 2 atmospheres (fluctuate between 1.5 atmospheres and 2 atmospheres), and the injection pressure of the water vapor port is about 1 atmosphere. Constant temperature at 120 degrees Celsius for 24 hours to obtain nano titanium dioxide powder materials with significantly improved dispersion, stability and transparency.
  • the main crystal phase of the titanium dioxide material obtained in Example 4 is anatase phase.
  • the product is mixed with water, and can also spontaneously disperse without stirring to form an aqueous dispersion in which nano titanium dioxide particles are stably suspended.
  • Figure 5 is an aqueous dispersion with a mass fraction of 5/1000 obtained after adding water to the nano-titania product obtained in this example, the dispersion has good monodispersity, and can form a relatively stable colloidal dispersion in the aqueous solution , with obvious Tyndall phenomenon; the nanoparticles are stably suspended, not easy to settle, and the solution is placed for more than 3 days without obvious stratification.
  • Figure 6 is an optical picture of the precursor titanium hydroxide suspension with a mass fraction of 5/1000 standing for 2 hours. It can be seen that there is an obvious layering phenomenon, and the suspension is unstable. It can be seen that this technology The suspension stability of the obtained product was increased by more than 36 times.
  • the light transmittance of the titanium dioxide material aqueous dispersion obtained in this embodiment 4 at a wavelength of 550 nanometers is 85%, compared with 2.5% of the light transmittance of the same concentration of the precursor titanium hydroxide suspension, and the transparency is improved by 34 times.
  • the specific experimental operation is as follows: take a small amount of the titanium dioxide material obtained in Example 1, prepare it into an aqueous dispersion with a mass fraction of 5/10,000, for comparison, and also prepare a precursor hydroxide with a mass fraction of 5/10,000. Titanium suspension; then respectively take the above dispersion in a 1 cm thick quartz cuvette, test the transmittance of the sample at a wavelength of 550 nm, and use pure water as a blank.
  • the precursor is an aggregate of nanoparticles of about 50 nanometers, with poor dispersion, which further shows that the precursor is easy to settle and stratify in water.
  • the dispersion degree of the titanium dioxide product obtained after the treatment by this technology has been significantly improved, and the dispersion degree has been increased by about 50 times.
  • the titanium dioxide product processed by this technology has been significantly improved in terms of dispersibility, dispersion stability, and transparency after dispersion, which will greatly expand the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
  • the advantages of the present invention are: (1) The technical method does not use any surface organic additive, which makes the application field of the nano titanium dioxide dispersion universal, and increases the application field and effect of the dispersion. (2) The processing temperature of the technical method is low, the operation steps are simple, and the price is low, which is favorable for large-scale industrialization and application.
  • the main crystal phase of the titanium dioxide material obtained in Example 5 is anatase phase and contains a trace amount of rutile phase.
  • This product is mixed with water, and can spontaneously disperse without stirring to form an aqueous dispersion in which nano-titanium dioxide particles are stably suspended, with obvious Tyndall phenomenon. Significant delamination occurred.
  • the precursor titanium hydroxide suspension was left standing for 2 hours, an obvious layering phenomenon appeared. It can be seen that the suspension stability of the product obtained by this technology has increased by more than 24 times.
  • the light transmittance of the titanium dioxide material aqueous dispersion obtained in this Example 5 at a wavelength of 550 nanometers is 67%, which is 27 times higher than that of the 2.5% light transmittance of the precursor titanium hydroxide suspension with the same concentration.
  • the experimental procedure is the same as that in Example 4.
  • the dispersion degree of the titanium dioxide material aqueous dispersion obtained in Example 5 is approximately 20 times higher. It can be seen that the titanium dioxide product processed by this technology has been significantly improved in terms of dispersibility, dispersion stability, and transparency after dispersion, which will greatly expand the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
  • amorphous nano-titanium dioxide particles weigh 10 grams of self-made amorphous nano-titanium dioxide particles and place them in a pressure-resistant anti-corrosion tube.
  • the preparation method of the amorphous nano-titanium dioxide particles is: slowly add an ethanol solution containing titanium isopropoxide dropwise to a pH value of 2 Hydrolyzed in nitric acid-ethanol aqueous solution, washed, separated and dried. Subsequently, the pressure-resistant anti-corrosion pipe was heated to 140 degrees Celsius, the pressure of the hydrogen chloride injection port in the pipe was kept unchanged at 2 atmospheres, and the temperature was kept at 140 degrees Celsius for 16 hours to obtain a water-phase monodispersion with significantly improved dispersion, stability and transparency. Nano titanium dioxide powder material.
  • the crystal phase of the titanium dioxide material obtained in Example 6 was an anatase phase.
  • This product is mixed with water, and can spontaneously disperse without stirring to form an aqueous dispersion in which nano-titanium dioxide particles are stably suspended, with obvious Tyndall phenomenon. Significant delamination occurred. For comparison, when the precursor suspension was left standing for 5 hours, an obvious stratification phenomenon appeared. It can be seen that the suspension stability of the product obtained by this technology has increased by more than 288 times.
  • the light transmittance of the titanium dioxide material aqueous dispersion obtained in Example 6 at a wavelength of 550 nanometers is 95%, compared with 6% of the light transmittance of the precursor suspension with the same concentration, the transparency is improved by 16 times.
  • the specific experiment Operation is the same as Example 4.
  • the dispersion degree of the titanium dioxide material aqueous dispersion obtained in Example 6 is increased by about 10 times. It can be seen that the titanium dioxide product processed by this technology has been significantly improved in terms of dispersibility, dispersion stability, and transparency after dispersion, which will greatly expand the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
  • the preparation method of the crystalline nano-titanium dioxide particles is as follows: slowly drop an ethanol solution containing titanium isopropoxide into a pH value of 2. Hydrolyzed in an aqueous nitric acid-ethanol solution, washed, separated and dried, and then annealed at 300 degrees Celsius for 3 hours, the crystalline phase is anatase phase.
  • the pressure-resistant anti-corrosion pipe was heated to 200 degrees Celsius, the pressure of the hydrogen chloride injection port in the pipe was kept constant at 5 atmospheres, and the injection pressure of the water vapor port was 5 atmospheres, and the temperature was kept at 200 degrees Celsius for 10 hours to obtain dispersion and stability.
  • Transparent and significantly improved nano titanium dioxide powder material was obtained.
  • the crystal phase of the titanium dioxide material obtained in Example 7 was an anatase phase.
  • This product is mixed with water, and can spontaneously disperse without stirring to form an aqueous dispersion in which nano-titanium dioxide particles are stably suspended, with obvious Tyndall phenomenon. Significant delamination occurred. For comparison, when the precursor suspension was left standing for 3 hours, an obvious stratification phenomenon appeared. It can be seen that the suspension stability of the product obtained by this technology has increased by more than 80 times.
  • the light transmittance of the titanium dioxide material aqueous dispersion obtained in Example 7 at a wavelength of 550 nanometers is 83%, which is 23 times higher than that of the 3.6% light transmittance of the precursor suspension with the same concentration.
  • the specific experiment Operation is the same as Example 4.
  • the dispersion degree of the titanium dioxide material aqueous dispersion obtained in Example 7 was increased by about 20 times. It can be seen that the titanium dioxide product processed by this technology has been significantly improved in terms of dispersibility, dispersion stability, and transparency after dispersion, which will greatly expand the application of titanium dioxide materials in the fields of ultraviolet absorption and aesthetics.
  • 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 de préparation de dioxyde de titane et une méthode d'amélioration de la dispersibilité du dioxyde de titane. L'invention concerne une méthode de préparation d'un oxyde de titane cristallisé à basse température, la méthode comprenant les étapes suivantes consistant à : (1) soumettre un composé de titane à des procédés d'hydrolyse, de séparation, de purification et de séchage pour obtenir de l'acide titanique hydraté ; (2) chauffer l'acide titanique hydraté à 100°C à 200°C ; et (3) introduire un gaz de chlorure d'hydrogène dans le système d'acide titanique hydraté chauffé et réaliser une réaction à pression constante pour obtenir un matériau de dioxyde de titane nanométrique cristallin. La méthode technique du dioxyde de titane cristallisé à basse température peut améliorer la méthode de synthèse par précipitation de dioxyde de titane nanométrique, et peut également améliorer les performances et le champ d'application de matériaux nanométriques de dioxyde de titane.
PCT/CN2021/104594 2020-07-06 2021-07-05 Méthode de préparation de dioxyde de titane et méthode d'amélioration de la dispersibilité du dioxyde de titane WO2022007764A1 (fr)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57123824A (en) * 1981-01-20 1982-08-02 Mitsubishi Metal Corp Preparation of rutile-type ultra-fine titanium oxide
JPH0967125A (ja) * 1995-08-30 1997-03-11 Showa Denko Kk 酸化チタン微粉末及びその製造法
KR20010025629A (ko) * 2001-01-12 2001-04-06 이종국 산처리에 의한 산화티탄 결정분말의 제조
JP2002060220A (ja) * 2000-08-17 2002-02-26 Sumitomo Chem Co Ltd ルチル型酸化チタン粉末の製造方法
CN1597534A (zh) * 2004-07-19 2005-03-23 南京大学 一种纳米金红石型二氧化钛的制法
CN101065325A (zh) * 2004-10-14 2007-10-31 托库森美国股份有限公司 纳米尺寸二氧化钛颗粒的合成方法
CN104098133A (zh) * 2014-07-02 2014-10-15 江苏恒智纳米科技有限公司 高效光催化剂-纳米二氧化钛水性胶体的制备方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57123824A (en) * 1981-01-20 1982-08-02 Mitsubishi Metal Corp Preparation of rutile-type ultra-fine titanium oxide
JPH0967125A (ja) * 1995-08-30 1997-03-11 Showa Denko Kk 酸化チタン微粉末及びその製造法
JP2002060220A (ja) * 2000-08-17 2002-02-26 Sumitomo Chem Co Ltd ルチル型酸化チタン粉末の製造方法
KR20010025629A (ko) * 2001-01-12 2001-04-06 이종국 산처리에 의한 산화티탄 결정분말의 제조
CN1597534A (zh) * 2004-07-19 2005-03-23 南京大学 一种纳米金红石型二氧化钛的制法
CN101065325A (zh) * 2004-10-14 2007-10-31 托库森美国股份有限公司 纳米尺寸二氧化钛颗粒的合成方法
CN104098133A (zh) * 2014-07-02 2014-10-15 江苏恒智纳米科技有限公司 高效光催化剂-纳米二氧化钛水性胶体的制备方法

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