A method for preparing highly dispersible titanium dioxide
Solid-liquid system is formed by sodium chloride and ascorbic acid, combined with silicon oxygen modification and alumina doping, the self-aggregation problem caused by the surfactivity of titanium dioxide is solved, and a high dispersion and stable preparation of titanium dioxide is achieved. It is suitable for industrial fields such as coatings, inks, papermaking, plastic rubber, chemical fibers and ceramics.
Patent Information
- Application Number
- CN202310642647.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-06-01
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2043-06-01
AI Technical Summary
The surface activity of existing titanium dioxide leads to self-aggregation, which is difficult to reach the particle size required for application, and the surface hydroxyl radicals are prone to resuscitation under light conditions, causing self-aggregation problems.
Sodium chloride colloidal particles barrier and ascorbic acid slightly soluble form a solid-liquid system, combined with silicon oxygen modification and alumina doping, forming an insulating shell layer, preventing hydroxyl radicals from being exposed, and reducing agglomeration through gradient cleaning and surface modification treatment.
It achieves high dispersion and stability of titanium dioxide, maintains excellent white properties, reduces self-aggregation under the influence of light, and improves the cleanliness and dispersion of the material.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of titanium dioxide, and particularly relates to a method for preparing highly dispersible titanium dioxide. Background Art
[0002] Titanium dioxide is an important inorganic chemical pigment, primarily composed of titanium dioxide. Titanium dioxide is produced via two processes: the sulfuric acid process and the chloride process. It has important applications in industries such as coatings, inks, papermaking, plastics and rubber, chemical fibers, and ceramics. my country's total titanium dioxide production capacity accounts for 30% of the world's total, making it the world's largest producer. In 2011, the country's total titanium dioxide production capacity reached approximately 2.6 million tons. Furthermore, my country has become the world's largest consumer of titanium dioxide. From 1999 to 2011, annual consumption increased from 248,000 tons to 1.65 million tons, achieving a compound annual growth rate of 17.11%, far exceeding GDP growth. With the continuous development of the titanium dioxide industry, quality requirements for titanium dioxide have continued to rise, and particle size requirements have become increasingly stringent. Titanium dioxide, primarily composed of titanium dioxide, contains a large number of hydroxyl groups on its surface, which can easily cause titanium dioxide to agglomerate, resulting in larger particles and making it difficult to meet application requirements. Summary of the Invention
[0003] In response to the problems in the prior art, the present invention provides a method for preparing highly dispersible titanium dioxide, which solves the problem of self-agglomeration caused by the surface activity of the existing titanium dioxide. The method utilizes the barrier of the colloidal particles of sodium chloride and the slight solubility of ascorbic acid to form a hydroxyl radical elimination reaction in a solid-liquid system, passivating the surface of the titanium dioxide and achieving good dispersibility.
[0004] In order to achieve the above technical objectives, the technical solution of the present invention is:
[0005] A method for preparing highly dispersible titanium dioxide comprises the following steps:
[0006] Step 1: Sodium chloride is added to ethanol and stirred evenly to form a colloidal liquid, and then titanium dioxide is added and ultrasonically dispersed for 20-30 minutes to obtain a mixed colloidal liquid. The concentration of sodium chloride in ethanol is 200-400 g / L, the stirring speed for uniform stirring is 300-500 r / min, the amount of titanium dioxide added is 50-70% of the mass of sodium chloride, the ultrasonic frequency of ultrasonic dispersion is 60-80 kHz, and the temperature is 20-30° C. This step utilizes the insolubility of sodium chloride in ethanol to form a colloidal liquid. At the same time, the colloidal liquid is homogeneous and can colloidalize the entire ethanol. Titanium dioxide is added to the colloidal liquid and ultrasonically dispersed to ensure that sodium chloride is wrapped on the surface of the titanium dioxide. Sodium chloride is used as a spacer to form a homogeneous dispersion of titanium dioxide, effectively preventing the agglomeration of the titanium dioxide itself.
[0007] Step 2: Mix ascorbic acid and ethanol aqueous solution and ball mill for 10-20 minutes to obtain a slurry, then slowly add the slurry to the mixed glue, and stir the reaction at a constant temperature to obtain a prefabricated slurry, wherein the mass ratio of ascorbic acid to ethanol aqueous solution is 5:1-2, and the volume proportion of ethanol in the ethanol aqueous solution is 93-95%, the mixing is mechanically stirred at 100-200r / min, the pressure of the ball milling treatment is 0.3-0.5MPa, and the temperature is 10-20°C; the addition rate of the slurry is 1-2g / min, and the amount of ascorbic acid added is 70-80% of the mass of titanium dioxide, the temperature of the constant temperature stirring reaction is 50-60°C, and the stirring speed is 200-300r / min; this step utilizes ascorbic acid to be slightly soluble in ethanol and water. The solubility of the slurry is used to form a mixed slurry, and the slurry is formed into fine crystals by ball milling. At the same time, the volume of water in the ethanol aqueous solution is not high, which effectively promotes the fine crystallization of ascorbic acid. Therefore, a small amount of ascorbic acid in the slurry is dissolved in the ethanol aqueous solution; the slurry is slowly added to the mixed colloid, and a small amount of ethanol aqueous solution is introduced into the entire system. The mixed colloid itself uses ethanol as a solvent, which forms a slightly soluble system for ascorbic acid, and can slowly dissolve and disperse it into the entire colloid. At the same time, the entry of water molecules stimulates the exposure of hydroxyl radicals on the surface of titanium dioxide. Under the action of temperature, the ascorbic acid dissolved in ethanol quickly eliminates the hydroxyl radicals. When the water molecules act on the surface of titanium dioxide, they also carry ascorbic acid to the surface of titanium dioxide, thereby achieving the effect of quickly removing free radicals on the surface of titanium dioxide;
[0008] Step 3, the prefabricated slurry is filtered to obtain a precipitate, which is then added to an ethanol aqueous solution and rapidly stirred. After filtering, it is repeatedly washed to obtain a white precipitate; the volume of water in the ethanol aqueous solution accounts for 10-20%, the concentration of the precipitate in the ethanol aqueous solution is 100-200g / L, the stirring speed of the rapid stirring is 2000-3000r / min, the ethanol aqueous solution is used for repeated washing, and the volume of distilled water in the ethanol aqueous solution accounts for 10-15%. This step removes the solvent in the slurry by means of suction filtration to form a mixed precipitate, and then the precipitate is stirred and dispersed in the ethanol aqueous solution. At this time, ascorbic acid and sodium chloride can be dissolved in the distilled water in the ethanol aqueous solution, achieving the effect of dissolving impurities. At this time, the ascorbic acid is dissolved in water and has excellent reducing properties. It can effectively inhibit the hydroxyl radicals on the surface of titanium dioxide, realize surface passivation of titanium dioxide, and prevent self-agglomeration of titanium dioxide; repeated washing with a low-water-content ethanol aqueous solution can effectively remove residual impurities in the titanium dioxide precipitate, thereby improving the cleanliness of titanium dioxide;
[0009] Step 4: Place the white precipitate in an ethanol-ether mixture and stir, then spray dry and deposit to obtain highly dispersible titanium dioxide. The volume ratio of ethanol to ether in the ethanol-ether mixture is 3:1-2, the stirring speed is 500-1000 r / min, the spray drying spray volume is 5-10 mL / min, and the spray area is 200-300 cm 2 , the temperature is 80-90°C; this step utilizes the characteristic that the ethanol and ether mixture does not contain distilled water to effectively prevent the formation of active groups on the surface of titanium dioxide, reduce the agglomeration problem of titanium dioxide, and at the same time, the spray drying method converts ethanol and ether into gas, and the titanium dioxide is precipitated to obtain uniformly dispersed titanium dioxide.
[0010] Furthermore, the main component of the titanium dioxide is titanium dioxide, which will form a certain excitation under light conditions, bringing about an increase in surface activity. Even if the above method removes the hydroxyl radicals on the surface of the titanium dioxide plate and realizes the passivation of the titanium dioxide surface, with the influence of environmental factors such as ultraviolet light, the hydroxyl radicals on its surface will slowly recover, resulting in a self-agglomeration problem. To solve this problem, the titanium dioxide needs to be surface modified, and the modification treatment is used to shield the surface of the titanium dioxide, eliminate the exposure of hydroxyl radicals, reduce the adsorption of hydroxyl radicals to the material, thereby reducing the self-agglomeration of titanium dioxide and maintaining the high dispersion state of titanium dioxide. The surface modification treatment method of the titanium dioxide includes the following steps: a1, adding titanium dioxide to ethanol and stirring evenly, and ball milling for 1-2h, then adding ethanol and ether mixture to expand the solution, and ultrasonically treating for 20-30min, filtering to obtain the crushed titanium dioxide, and the mass ratio of the titanium dioxide to ethanol is 5:2-3 , the stirring speed for uniform stirring is 200-300r / min, the ball milling pressure for ball milling is 0.3-0.5MPa, and the temperature is 10-20°C; the volume ratio of ethanol to ether in the ethanol-ether mixture is 5:3-5, the dissolution multiple is 10-20, the frequency of ultrasonic treatment is 60-80kHz, and the temperature is 5-10°C; this step utilizes the insolubility of ethanol in titanium dioxide to form a wet ball milling treatment of particles, disperses the self-agglomerated particles of titanium dioxide, and obtains a uniformly dispersed preliminary slurry. Secondly, this step utilizes the dissolution of the ethanol-ether mixture to disperse the entire solution, and then at low temperature Further dispersing the slurry in ultrasound can not only improve the permeability of ethanol and ether, accelerate the further dispersion of self-agglomerated titanium dioxide, increase the reduction of titanium dioxide particles, but also effectively prevent the self-agglomeration of titanium dioxide; a2, adding the crushed titanium dioxide into the reactor and letting it stand for 10-20 minutes, and purging it with dry nitrogen to obtain titanium dioxide containing a liquid film; the atmosphere in the reactor is a mixed atmosphere of nitrogen and ethanol vapor, and the volume proportion of ethanol in the mixed atmosphere is 20-30%, and the standing temperature is 10-20°C; the purging speed is 5-10mL / min, and the temperature is 40-50°C ; This step utilizes the good film-forming property of ethanol in the mixed atmosphere, and the titanium dioxide itself has a certain adsorption property, which can adsorb ethanol molecules on the surface of titanium dioxide, and the gas has good permeability, completely covering the surface of titanium dioxide to form a preliminary liquid film system. During the dry nitrogen purge process, the nitrogen carries away the ethanol vapor in the air and maintains the stability of the ethanol liquid film; a3, trichloromethylsilane is added to ether and stirred evenly to form a dissolving solution, and then the dissolving solution is sprayed into the reactor containing the titanium dioxide containing the liquid film, and allowed to stand for 10-20 minutes, and the nitrogen purge is performed to obtain the pre-coated titanium dioxide;The concentration of trichloromethylsilane in diethyl ether is 10-20 g / L, the stirring speed for uniform stirring is 200-400 r / min, the temperature of the spray is 68-72° C., the temperature of the nitrogen purge is 65-70° C., and the purge speed is 20-30 mL / min. This step utilizes the solubility of the ethanol liquid film in diethyl ether to dissolve a certain amount of diethyl ether vapor, and utilizes the dissolved diethyl ether to absorb trichloromethylsilane in the air to obtain a surface liquid film structure, wherein the liquid film contains diethyl ether, ethanol and methyltrichlorosilane; a4, placing the pre-coated titanium dioxide in a reactor and allowing it to stand for 20-30 minutes, and then sintering it at a constant temperature for 20-30 minutes to obtain silicon dioxide. Oxygen-modified titanium dioxide, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10-15:1, the standing temperature is 50-70°C, and the temperature of the constant temperature sintering treatment is 120-150°C; this step utilizes the water vapor of the mixed atmosphere system to enter the ethanol and form a hydrolysis reaction with the trichloromethylsilane in the ethanol, and the hydrolysis reaction obtains trihydroxymethylsilane. During the constant temperature sintering process, the trihydroxymethylsilane forms a condensation reaction, resulting in the formation of a loose silica shell on the surface of the titanium dioxide; at this time, the ethanol and ether are converted into steam and removed; a5, the silica-modified titanium dioxide is placed in water and fully stirred, taken out and dried, and then placed In the middle section of the reactor, aluminum isopropoxide vapor is introduced and allowed to stand for 10-20 minutes, and then the temperature is rapidly reduced to obtain doped silicon-oxygen modified titanium dioxide. The concentration of the silicon-oxygen modified titanium dioxide in water is 100-300 g / L, the stirring speed is 200-300 r / min, and the standing temperature is 140-150° C. The volume proportion of the aluminum isopropoxide vapor in the standing atmosphere is 10-15%, and the temperature of the rapid cooling is 100-105° C. This step utilizes the loose silicon-oxygen structure on the surface of the silicon-oxygen modified titanium dioxide to promote the activity of the exposed surface of the titanium dioxide through water molecules, forming aluminum isopropoxide doping in the penetration of aluminum isopropoxide vapor, and quickly converting it into Aluminum isopropoxide particles are prepared to obtain aluminum isopropoxide deposition. At the same time, a small amount of water molecules will still remain in the silicon-oxygen modified titanium dioxide after drying. The residual water molecules will adsorb aluminum isopropoxide in the aluminum isopropoxide vapor and hydrolyze and convert the aluminum isopropoxide; a6, placing the doped silicon-oxygen modified titanium dioxide in a reactor and letting it stand for 20-30 minutes, and obtaining aluminum oxide-silicon-oxygen modified titanium dioxide after high-temperature sintering treatment, wherein the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor in the mixed atmosphere is 10:1-2, the standing temperature is 90-100° C., and the temperature of the high-temperature sintering treatment is 800-1000° C.; the sintering time is 1-2 hours;This step uses a water-containing atmosphere to react with doped silicon-oxygen modified titanium dioxide to form a hydrolysis reaction system, converting aluminum isopropylate into aluminum hydroxide, and this conversion is an in-situ hydrolysis reaction. The sintering treatment in a high-temperature system can convert aluminum hydroxide into aluminum oxide. This process forms a surface treatment on titanium dioxide, which forms a composite shell of silicon oxide and aluminum oxide on the surface of titanium dioxide, forming a good wrapping system for titanium dioxide. Based on the small amount of deposition of trichloromethylsilane and aluminum isopropylate, a very thin shell structure is formed on the surface of titanium dioxide, and the shell is based on silicon oxide as the framework and aluminum oxide as the doping structure. The surface of the titanium dioxide with this core-shell structure is shielded by the doping type of aluminum oxide, reducing the impact of light on titanium dioxide. At the same time, both silicon oxide and aluminum oxide are insulating, which can effectively prevent the influence of hydroxyl radicals on the surface of titanium dioxide and ensure the dispersibility of the material itself.
[0011] Furthermore, the surface modified titanium dioxide is pretreated before use, and the pretreatment steps include: b1, adding alumina-silica modified titanium dioxide to ethanol and ultrasonically treating it for 20-30 minutes, filtering to obtain preliminarily washed alumina-silica modified titanium dioxide, the mass ratio of the alumina-silica modified titanium dioxide to ethanol is 2:2-3, the ultrasonic frequency of the ultrasonic treatment is 50-70kHz, and the temperature is 20-30°C; this step uses ultrasound to treat the alumina-silica modified titanium dioxide, and uses the permeability and film-forming properties of ethanol to form a surface coverage of the alumina-silica modified titanium dioxide, thereby achieving a specific surface coverage of the alumina-silica modified titanium dioxide; b2, adding alumina-silica modified titanium dioxide to ethanol aqueous solution and ultrasonically treating it for 20-30 minutes, filtering to obtain prefabricated alumina-silica modified titanium dioxide, the volume proportion of ethanol in the ethanol aqueous solution is 60-70%, and the alumina-silica modified titanium dioxide in the ethanol aqueous solution is 10%. The concentration is 40-70g / L, the ultrasonic frequency of the ultrasonic treatment is 70-80kHz, and the temperature is 40-60℃; this step uses high-frequency ultrasonic vibration to send the liquid to the specific surface of the alumina-silicone modified titanium dioxide, and cooperates with the pre-formation of the ethanol liquid film to ensure that distilled water is formed on the specific surface of the alumina-silicone modified titanium dioxide to achieve a water washing effect; b3, add the alumina-silicone modified titanium dioxide to the ethanol ether mixture and perform low-temperature ultrasonic treatment for 40-50min, filter and collect Washing with an ethanol-ether mixture and spray drying to obtain clean alumina-silicone modified titanium dioxide, wherein the volume ratio of ethanol to ether in the ethanol-ether mixture is 3:2-3, the concentration of the alumina-silicone modified titanium dioxide in the ethanol-ether mixture is 40-70 g / L, the ultrasonic frequency of the low-temperature ultrasound is 70-80 kHz, the temperature is 5-10°C; the spray drying temperature is 80-90°C, the spray volume is 10-20 mL / min, and the spray area is 100 cm 2This pre-treatment uses ethanol as a film-forming agent and wetting agent to form a liquid film on the specific surface of the alumina-silicone modified titanium dioxide. This helps ether and water form a permeable liquid film on the surface of the alumina-silicone modified titanium dioxide, better adhering to the specific surface of the alumina-silicone modified titanium dioxide, thereby achieving a surface cleaning effect, solving the problem of surface impurities deposition and adhesion, and ensuring the cleanliness of the titanium dioxide raw materials.
[0012] It can be seen from the above description that the present invention has the following advantages:
[0013] 1. The present invention solves the problem of self-agglomeration caused by the surface activity of existing titanium dioxide. It utilizes the barrier of colloidal particles of sodium chloride and the slight solubility of ascorbic acid to form a hydroxyl radical elimination reaction in a solid-liquid system, passivating the surface of titanium dioxide and having good dispersibility.
[0014] 2. The present invention utilizes silicon oxide modification in combination with aluminum oxide doping to form an insulating shell protective structure, which not only can seal the surface of titanium dioxide and reduce the generation and exposure of hydroxyl radicals, but also the inherent white color of aluminum oxide and the transparency of silicon oxide materials ensure that titanium dioxide still exhibits excellent white performance.
[0015] 3. The present invention utilizes a gradient cleaning method to remove impurities from the surface of titanium dioxide, which can not only remove physically deposited impurities, but also remove adhesive impurities. At the same time, ethanol acts as a wetting film to form a film-forming wetting structure system on the specific surface, achieving a high-quality wetting effect, enhancing the rapid diffusion of ether and water, and reducing surface bubbles. DETAILED DESCRIPTION
[0016] The present invention is described in detail with reference to the embodiments, but no limitation is imposed on the claims of the present invention.
[0017] Example 1
[0018] A method for preparing highly dispersible titanium dioxide comprises the following steps:
[0019] Step 1, titanium dioxide surface treatment: The method for surface modification of titanium dioxide comprises the following steps: a1, adding titanium dioxide to ethanol and stirring evenly, and ball milling for 1 hour, then adding ethanol and ether mixture to expand the solution, and ultrasonic treatment for 20 minutes, filtering to obtain crushed titanium dioxide, wherein the mass ratio of titanium dioxide to ethanol is 5:2, the stirring speed for uniform stirring is 200r / min, the ball milling pressure for ball milling is 0.3MPa, and the temperature is 10°C; the volume ratio of ethanol to ether in the ethanol and ether mixture is 5:3, the expansion multiple is 10, the ultrasonic treatment frequency is 60kHz, and the temperature is 5°C; a2, crushing the titanium dioxide Titanium dioxide is added to a reactor and allowed to stand for 10 minutes, and then purged with dry nitrogen to obtain titanium dioxide containing a liquid film; the atmosphere in the reactor is a mixed atmosphere of nitrogen and ethanol vapor, and the volume proportion of ethanol in the mixed atmosphere is 20%, and the standing temperature is 10°C; the purging speed is 5 mL / min, and the temperature is 40°C; a3, trichloromethylsilane is added to ether and stirred evenly to form a dissolving solution, and then the dissolving solution is sprayed into the reactor containing the titanium dioxide containing the liquid film, and the reaction mixture is allowed to stand for 10 minutes, and nitrogen is purged to obtain pre-coated titanium dioxide; the concentration of trichloromethylsilane in ether is 10 g / L, and the stirring speed for stirring evenly is 200 r / mi n, the temperature of the spray is 68 ° C, the temperature of the nitrogen purge is 65 ° C, and the purge rate is 20 mL / min; a4, the pre-coated titanium dioxide is placed in a reactor and allowed to stand for 20 minutes, and then sintered at a constant temperature for 20 minutes to obtain silicon-oxygen modified titanium dioxide, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10:1, the standing temperature is 50 ° C, and the temperature of the constant temperature sintering treatment is 120 ° C; a5, the silicon-oxygen modified titanium dioxide is placed in water and fully stirred, taken out and dried, and then placed in the middle of the reactor, and isopropyl alcohol aluminum vapor is introduced and allowed to stand for 10 minutes, and the doped silicon-oxygen titanium dioxide is obtained after rapid cooling. Modified titanium dioxide, wherein the concentration of the silicon-oxygen modified titanium dioxide in water is 100 g / L, the stirring speed is 200 r / min, and the standing temperature is 140° C.; the volume proportion of the aluminum isopropoxide vapor in the standing atmosphere is 10%, and the temperature of the rapid cooling is 100° C.; a6, placing the doped silicon-oxygen modified titanium dioxide in a reactor and standing for 20 minutes, and obtaining aluminum oxide-silicon-oxygen modified titanium dioxide after high-temperature sintering treatment, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor in the mixed atmosphere is 10:1, the standing temperature is 90° C., the temperature of the high-temperature sintering treatment is 800° C.; and the sintering time is 1 hour;
[0020] Step 2, the titanium dioxide is pre-treated before use, and the pre-treatment steps include: b1, adding alumina-silicone modified titanium dioxide to ethanol and ultrasonically treating it for 20 minutes, filtering to obtain preliminarily washed alumina-silicone modified titanium dioxide, wherein the mass ratio of the alumina-silicone modified titanium dioxide to ethanol is 2:2, the ultrasonic frequency of the ultrasonic treatment is 50kHz, and the temperature is 20°C; b2, adding alumina-silicone modified titanium dioxide to ethanol aqueous solution and ultrasonically treating it for 20 minutes, filtering to obtain prefabricated alumina-silicone modified titanium dioxide, wherein the volume proportion of ethanol in the ethanol aqueous solution is 60%, and the alumina-silicone modified titanium dioxide in the ethanol aqueous solution is 2:2. The concentration of the aluminum oxide-silicone modified titanium dioxide is 40 g / L, the ultrasonic frequency of the ultrasonic treatment is 70 kHz, and the temperature is 40 ° C; b3, adding the aluminum oxide-silicone modified titanium dioxide to an ethanol-ether mixture and ultrasonically treating it at low temperature for 40 minutes, filtering and washing with an ethanol-ether mixture, and spray drying to obtain a clean aluminum oxide-silicone modified titanium dioxide, wherein the volume ratio of ethanol to ether in the ethanol-ether mixture is 3:2, the concentration of the aluminum oxide-silicone modified titanium dioxide in the ethanol-ether mixture is 40 g / L, the ultrasonic frequency of the low-temperature ultrasonic treatment is 70 kHz, and the temperature is 5 ° C; the spray drying temperature is 80 ° C, the spray volume is 10 mL / min, and the spray area is 100 cm 2 ;
[0021] Step 3: adding sodium chloride to ethanol and stirring evenly to form a colloidal solution, then adding titanium dioxide and ultrasonically dispersing for 20 minutes to obtain a mixed colloidal solution, wherein the concentration of sodium chloride in ethanol is 200 g / L, the stirring speed for uniform stirring is 300 r / min, the amount of titanium dioxide added is 50% of the mass of sodium chloride, the ultrasonic frequency of ultrasonic dispersion is 60 kHz, and the temperature is 20°C;
[0022] Step 4, ascorbic acid and ethanol aqueous solution are mixed and ball-milled for 10 minutes to obtain a slurry, and then the slurry is slowly added to the mixed glue, and the reaction is stirred at a constant temperature to obtain a prefabricated slurry, the mass ratio of ascorbic acid to ethanol aqueous solution is 5:1, and the volume proportion of ethanol in the ethanol aqueous solution is 93%, the mixing is mechanically stirred at 100 r / min, the pressure of the ball milling treatment is 0.3 MPa, and the temperature is 10°C; the addition rate of the slurry is 1 g / min, and the amount of ascorbic acid added is 70% of the mass of titanium dioxide, the temperature of the constant temperature stirring reaction is 50°C, and the stirring speed is 200 r / min;
[0023] Step 5: Filter the prefabricated slurry to obtain a precipitate, then add it to an ethanol aqueous solution and rapidly stir it, filter it, and repeatedly wash it to obtain a white precipitate; the volume ratio of water in the ethanol aqueous solution is 10%, the concentration of the precipitate in the ethanol aqueous solution is 100 g / L, the stirring speed of the rapid stirring is 2000 r / min, and the repeated washing uses an ethanol aqueous solution, and the volume ratio of distilled water in the ethanol aqueous solution is 10%;
[0024] Step 6: Place the white precipitate in an ethanol-ether mixture and stir, then spray dry and deposit to obtain highly dispersible titanium dioxide. The volume ratio of ethanol to ether in the ethanol-ether mixture is 3:1, the stirring speed is 500 r / min, the spray drying spray volume is 5 mL / min, and the spray area is 200 cm 2 , the temperature is 80℃.
[0025] Example 2
[0026] A method for preparing highly dispersible titanium dioxide comprises the following steps:
[0027] Step 1, titanium dioxide surface treatment: The method for surface modification of titanium dioxide comprises the following steps: a1, adding titanium dioxide to ethanol, stirring evenly, and ball milling for 2 hours, then adding ethanol and ether mixture to expand the solution, and ultrasonic treatment for 30 minutes, filtering to obtain crushed titanium dioxide, wherein the mass ratio of titanium dioxide to ethanol is 5:3, the stirring speed for uniform stirring is 300r / min, the ball milling pressure for ball milling is 0.5MPa, and the temperature is 20°C; the volume ratio of ethanol to ether in the ethanol and ether mixture is 5:5, the expansion multiple is 20, the ultrasonic treatment frequency is 80kHz, and the temperature is 10°C; a2, crushing the titanium dioxide Titanium dioxide is added to a reactor and allowed to stand for 20 minutes, and then purged with dry nitrogen to obtain titanium dioxide containing a liquid film; the atmosphere in the reactor is a mixed atmosphere of nitrogen and ethanol vapor, and the volume proportion of ethanol in the mixed atmosphere is 30%, and the standing temperature is 20°C; the purging speed is 10 mL / min, and the temperature is 50°C; a3, trichloromethylsilane is added to ether and stirred evenly to form a dissolving solution, and then the dissolving solution is sprayed into the reactor containing the titanium dioxide containing the liquid film, and the reaction mixture is allowed to stand for 20 minutes, and nitrogen is purged to obtain pre-coated titanium dioxide; the concentration of trichloromethylsilane in ether is 20 g / L, and the stirring speed for stirring evenly is 400 r / mi n, the temperature of the spray is 72 ° C, the temperature of the nitrogen purge is 70 ° C, and the purge rate is 30 mL / min; a4, the pre-coated titanium dioxide is placed in a reactor and allowed to stand for 30 minutes, and then sintered at a constant temperature for 30 minutes to obtain silicon-oxygen modified titanium dioxide, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 15:1, the standing temperature is 70 ° C, and the constant temperature sintering temperature is 150 ° C; a5, the silicon-oxygen modified titanium dioxide is placed in water and fully stirred, taken out and dried, and then placed in the middle of the reactor, and isopropyl alcohol aluminum vapor is introduced and allowed to stand for 20 minutes, and the doped silicon-oxygen modified titanium dioxide is obtained after rapid cooling. a6, placing the doped silica-modified titanium dioxide in a reactor and allowing it to stand for 30 minutes, and subjecting it to high-temperature sintering treatment to obtain alumina-silica-modified titanium dioxide, wherein the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor in the mixed atmosphere is 10:2, the standing temperature is 100° C., the temperature of the high-temperature sintering treatment is 1000° C., and the sintering time is 2 hours;
[0028] Step 2, titanium dioxide is pretreated before use, and the pretreatment steps include: b1, adding alumina-silicone modified titanium dioxide to ethanol and ultrasonically treating it for 30 minutes, filtering to obtain preliminarily washed alumina-silicone modified titanium dioxide, wherein the mass ratio of the alumina-silicone modified titanium dioxide to ethanol is 2:3, the ultrasonic frequency of the ultrasonic treatment is 70kHz, and the temperature is 30°C; b2, adding alumina-silicone modified titanium dioxide to ethanol aqueous solution and ultrasonically treating it for 30 minutes, filtering to obtain prefabricated alumina-silicone modified titanium dioxide, wherein the volume proportion of ethanol in the ethanol aqueous solution is 70%, and the alumina-silicone modified titanium dioxide in the ethanol aqueous solution is 50%. The concentration is 70g / L, the ultrasonic frequency of the ultrasonic treatment is 80kHz, and the temperature is 60℃; b3, adding the aluminum oxide-silicone modified titanium dioxide to an ethanol-ether mixture and performing low-temperature ultrasonic treatment for 50min, filtering and washing with an ethanol-ether mixture, and spray drying to obtain a clean aluminum oxide-silicone modified titanium dioxide, wherein the volume ratio of ethanol to ether in the ethanol-ether mixture is 3:3, the concentration of the aluminum oxide-silicone modified titanium dioxide in the ethanol-ether mixture is 70g / L, the ultrasonic frequency of the low-temperature ultrasonic treatment is 80kHz, and the temperature is 10℃; the spray drying temperature is 90℃, the spray volume is 20mL / min, and the spray area is 100cm 2 ;
[0029] Step 3: adding sodium chloride to ethanol and stirring evenly to form a colloidal solution, then adding titanium dioxide and ultrasonically dispersing for 30 minutes to obtain a mixed colloidal solution, wherein the concentration of sodium chloride in ethanol is 400 g / L, the stirring speed for uniform stirring is 500 r / min, the amount of titanium dioxide added is 70% of the mass of sodium chloride, the ultrasonic frequency of ultrasonic dispersion is 80 kHz, and the temperature is 30°C;
[0030] Step 4, ascorbic acid and ethanol aqueous solution are mixed and ball milled for 20 minutes to obtain a slurry, and then the slurry is slowly added to the mixed glue, and the reaction is stirred at a constant temperature to obtain a prefabricated slurry, the mass ratio of ascorbic acid to ethanol aqueous solution is 5:2, and the volume proportion of ethanol in the ethanol aqueous solution is 95%, the mixing is mechanically stirred at 200r / min, the pressure of the ball milling treatment is 0.5MPa, and the temperature is 20°C; the addition rate of the slurry is 2g / min, and the amount of ascorbic acid added is 70-80% of the mass of titanium dioxide, the temperature of the constant temperature stirring reaction is 60°C, and the stirring speed is 300r / min;
[0031] Step 5: Filter the prefabricated slurry to obtain a precipitate, then add it to an ethanol aqueous solution and rapidly stir it, filter it, and repeatedly wash it to obtain a white precipitate; the volume ratio of water in the ethanol aqueous solution is 20%, the concentration of the precipitate in the ethanol aqueous solution is 200 g / L, the stirring speed of the rapid stirring is 3000 r / min, and the repeated washing uses an ethanol aqueous solution, and the volume ratio of distilled water in the ethanol aqueous solution is 15%;
[0032] Step 6: Place the white precipitate in an ethanol-ether mixture and stir, then spray dry and deposit to obtain highly dispersible titanium dioxide. The volume ratio of ethanol to ether in the ethanol-ether mixture is 3:2, the stirring speed is 1000 r / min, the spray drying spray volume is 10 mL / min, and the spray area is 300 cm 2 , the temperature is 90℃.
[0033] Example 3
[0034] A method for preparing highly dispersible titanium dioxide comprises the following steps:
[0035] Step 1, titanium dioxide surface treatment: The method for surface modification of titanium dioxide comprises the following steps: a1, adding titanium dioxide to ethanol and stirring evenly, and ball milling for 2h, then adding ethanol and ether mixture to expand the solution, and ultrasonic treatment for 25min, filtering to obtain crushed titanium dioxide, wherein the mass ratio of titanium dioxide to ethanol is 5:2, the stirring speed for uniform stirring is 250r / min, the ball milling pressure for ball milling is 0.4MPa, and the temperature is 15°C; the volume ratio of ethanol to ether in the ethanol and ether mixture is 5:4, the expansion multiple is 15, the ultrasonic treatment frequency is 70kHz, and the temperature is 8°C; a2, crushing the titanium dioxide Titanium dioxide is added to a reactor and allowed to stand for 15 minutes, and then purged with dry nitrogen to obtain titanium dioxide containing a liquid film; the atmosphere in the reactor is a mixed atmosphere of nitrogen and ethanol vapor, and the volume proportion of ethanol in the mixed atmosphere is 25%, and the standing temperature is 15°C; the purging speed is 8 mL / min, and the temperature is 45°C; a3, trichloromethylsilane is added to ether and stirred evenly to form a dissolving solution, and then the dissolving solution is sprayed into the reactor containing the titanium dioxide containing the liquid film, and allowed to stand for 15 minutes, and purged with nitrogen to obtain pre-coated titanium dioxide; the concentration of the trichloromethylsilane in the ether is 15 g / L, and the stirring speed for stirring evenly is 300 r / min , the temperature of the spray is 70°C, the temperature of the nitrogen purge is 70°C, and the purge rate is 25mL / min; a4, the pre-coated titanium dioxide is placed in a reactor and allowed to stand for 25min, and then sintered at a constant temperature for 25min to obtain silicon-oxygen modified titanium dioxide, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 12:1, the standing temperature is 60°C, and the constant temperature sintering temperature is 140°C; a5, the silicon-oxygen modified titanium dioxide is placed in water and fully stirred, taken out and dried, and then placed in the middle section of the reactor, and isopropyl alcohol aluminum vapor is introduced and allowed to stand for 15min, and the doped silicon-oxygen modified titanium dioxide is obtained after rapid cooling. Titanium dioxide, the concentration of the silicon-oxygen modified titanium dioxide in water is 200 g / L, the stirring speed is 250 r / min, and the standing temperature is 145° C.; the volume proportion of the aluminum isopropoxide vapor in the standing atmosphere is 12%, and the temperature of the rapid cooling is 100° C.; a6, placing the doped silicon-oxygen modified titanium dioxide in a reactor and standing for 20-30 minutes, and obtaining aluminum oxide-silicon-oxygen modified titanium dioxide after high-temperature sintering treatment, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor in the mixed atmosphere is 10:1, the standing temperature is 95° C., the temperature of the high-temperature sintering treatment is 900° C.; the sintering time is 2 hours;
[0036] Step 2, the titanium dioxide is pre-treated before use, and the pre-treatment steps include: b1, adding alumina-silicone modified titanium dioxide to ethanol and ultrasonically treating it for 25 minutes, filtering to obtain preliminarily washed alumina-silicone modified titanium dioxide, wherein the mass ratio of the alumina-silicone modified titanium dioxide to ethanol is 2:3, the ultrasonic frequency of the ultrasonic treatment is 60kHz, and the temperature is 26°C; b2, adding alumina-silicone modified titanium dioxide to ethanol aqueous solution and ultrasonically treating it for 26 minutes, filtering to obtain prefabricated alumina-silicone modified titanium dioxide, wherein the volume proportion of ethanol in the ethanol aqueous solution is 66%, and the alumina-silicone modified titanium dioxide in the ethanol aqueous solution is 2:3. The concentration of the aluminum oxide-silicone modified titanium dioxide is 60 g / L, the ultrasonic frequency of the ultrasonic treatment is 76 kHz, and the temperature is 50 ° C; b3, adding the aluminum oxide-silicone modified titanium dioxide to an ethanol-ether mixture and ultrasonically treating it at low temperature for 45 minutes, filtering and washing with an ethanol-ether mixture, and spray drying to obtain a clean aluminum oxide-silicone modified titanium dioxide, wherein the volume ratio of ethanol to ether in the ethanol-ether mixture is 3:2, the concentration of the aluminum oxide-silicone modified titanium dioxide in the ethanol-ether mixture is 60 g / L, the ultrasonic frequency of the low-temperature ultrasonic treatment is 75 kHz, and the temperature is 8 ° C; the spray drying temperature is 85 ° C, the spray volume is 15 mL / min, and the spray area is 100 cm 2 ;
[0037] Step 3: adding sodium chloride to ethanol and stirring evenly to form a colloidal solution, then adding titanium dioxide and ultrasonically dispersing for 25 minutes to obtain a mixed colloidal solution, wherein the concentration of sodium chloride in ethanol is 300 g / L, the stirring speed for uniform stirring is 400 r / min, the amount of titanium dioxide added is 60% of the mass of sodium chloride, the ultrasonic frequency of ultrasonic dispersion is 70 kHz, and the temperature is 25°C;
[0038] Step 4, ascorbic acid and ethanol aqueous solution are mixed and ball milled for 15 minutes to obtain a slurry, and then the slurry is slowly added to the mixed glue, and the reaction is stirred at a constant temperature to obtain a prefabricated slurry, the mass ratio of ascorbic acid to ethanol aqueous solution is 5:1-2, and the volume proportion of ethanol in the ethanol aqueous solution is 94%, the mixing is mechanically stirred at 200r / min, the ball milling pressure is 0.4MPa, and the temperature is 15°C; the slurry is added at a rate of 2g / min, and the amount of ascorbic acid added is 75% of the mass of titanium dioxide, the temperature of the constant temperature stirring reaction is 55°C, and the stirring speed is 250r / min;
[0039] Step 5: Filtering the prefabricated slurry to obtain a precipitate, then adding it to an ethanol aqueous solution and rapidly stirring it, filtering it, and repeatedly washing it to obtain a white precipitate; the volume ratio of water in the ethanol aqueous solution is 15%, the concentration of the precipitate in the ethanol aqueous solution is 150 g / L, the stirring speed of the rapid stirring is 2500 r / min, and the repeated washing uses an ethanol aqueous solution, and the volume ratio of distilled water in the ethanol aqueous solution is 13%;
[0040] Step 6: Place the white precipitate in an ethanol-ether mixture and stir, then spray dry and deposit to obtain highly dispersible titanium dioxide. The volume ratio of ethanol to ether in the ethanol-ether mixture is 3:2, the stirring speed is 800 r / min, the spray drying spray volume is 8 mL / min, and the spray area is 250 cm 2 , the temperature is 85℃.
[0041] Example 4
[0042] A method for preparing highly dispersible titanium dioxide comprises the following steps:
[0043] Step 1: Sodium chloride is added to ethanol and stirred to form a colloidal solution, and then titanium dioxide is added and ultrasonically dispersed for 25 minutes to obtain a mixed colloidal solution. The concentration of sodium chloride in ethanol is 300 g / L, the stirring speed for uniform stirring is 400 r / min, the amount of titanium dioxide added is 60% of the mass of sodium chloride, the ultrasonic frequency of ultrasonic dispersion is 70 kHz, and the temperature is 25°C;
[0044] Step 2: Ascorbic acid and an ethanol aqueous solution are mixed and ball-milled for 15 minutes to obtain a slurry, and then the slurry is slowly added to the mixed glue solution, and the reaction is stirred at a constant temperature to obtain a prefabricated slurry, wherein the mass ratio of ascorbic acid to ethanol aqueous solution is 5:1-2, and the volume proportion of ethanol in the ethanol aqueous solution is 94%. The mixing is mechanically stirred at 200 r / min, the pressure of the ball milling treatment is 0.4 MPa, and the temperature is 15°C; the addition rate of the slurry is 2 g / min, and the amount of ascorbic acid added is 75% of the mass of titanium dioxide. The temperature of the constant temperature stirring reaction is 55°C and the stirring speed is 250 r / min;
[0045] Step 3: Filtering the prefabricated slurry to obtain a precipitate, then adding it to an ethanol aqueous solution and rapidly stirring it, filtering it, and repeatedly washing it to obtain a white precipitate; the volume ratio of water in the ethanol aqueous solution is 15%, the concentration of the precipitate in the ethanol aqueous solution is 150 g / L, the stirring speed of the rapid stirring is 2500 r / min, and the repeated washing uses an ethanol aqueous solution, and the volume ratio of distilled water in the ethanol aqueous solution is 13%;
[0046] Step 4: Place the white precipitate in an ethanol-ether mixture and stir, then spray dry and deposit to obtain highly dispersible titanium dioxide. The volume ratio of ethanol to ether in the ethanol-ether mixture is 3:2, the stirring speed is 800 r / min, the spray drying spray volume is 8 mL / min, and the spray area is 250 cm 2 , the temperature is 85℃.
[0047] Water dispersibility test
[0048] Using Examples 1-4 as the test samples, water dispersibility test was performed
[0049] The water dispersibility test was conducted using a sedimentation method with a sedimentation time of 5 hours. The test results are as follows:
[0050] Example 1 Example 2 Example 3 Example 4 Water dispersibility 98.6% 99.1% 98.8% 95.6%
[0051] Before the water dispersibility test, the products of Examples 1-4 were irradiated with UV light for 10 hours to obtain the samples to be tested after irradiation. The water dispersibility test results are as follows:
[0052] Example 1 Example 2 Example 3 Example 4 Water dispersibility 96.3% 97.3% 96.9% 73.1%
[0053] In comparison with the above, the titanium dioxide provided by the present technical solution has good high dispersibility, can form a homogeneous dispersion in water, and has good dispersibility even after exposure to light.
[0054] It is understood that the above specific description of the present invention is only used to illustrate the present invention and is not limited to the technical solutions described in the embodiments of the present invention. Those skilled in the art should understand that the present invention can still be modified or replaced with equivalents to achieve the same technical effects; as long as the use requirements are met, they are all within the scope of protection of the present invention.
Claims
1. A method for preparing highly dispersible titanium dioxide, characterized in that: The steps include: Step 1, titanium dioxide surface treatment: The titanium dioxide surface modification method comprises the following steps: a1, adding titanium dioxide to ethanol, stirring uniformly, and ball milling for 1-2 hours, then adding a mixture of ethanol and ether to dissolve it, and ultrasonically treating it for 20-30 minutes, filtering to obtain crushed titanium dioxide, wherein the mass ratio of titanium dioxide to ethanol is 5:2-3, the stirring speed for uniform stirring is 200-300 r / min, and the ball milling pressure for ball milling is 0.3-0.5MPa, temperature is 10-20°C; the volume ratio of ethanol and ether in the ethanol-ether mixture is 5:3-5, the dissolution multiple is 10-20, the frequency of ultrasonic treatment is 60-80kHz, and the temperature is 5-10°C; a2, adding the crushed titanium dioxide into the reactor and standing for 10-20min, purging with dry nitrogen to obtain titanium dioxide containing a liquid film; the atmosphere in the reactor is a mixed atmosphere of nitrogen and ethanol vapor, and the volume proportion of ethanol in the mixed atmosphere is 20-30%, and the standing temperature is 10-20°C; the purging speed is 5-10mL / min, and the temperature is 40- 50℃; a3, add trichloromethylsilane to ether and stir evenly to form a dissolving solution, then spray the dissolving solution into the reactor containing the titanium dioxide containing the liquid film, let it stand for 10-20 minutes, and purge with nitrogen to obtain pre-coated titanium dioxide; the concentration of the trichloromethylsilane in the ether is 10-20g / L, the stirring speed for uniform stirring is 200-400r / min, the temperature of the spray is 68-72℃, the temperature of the nitrogen purge is 65-70℃, and the purge speed is 20-30mL / min; a4, put the pre-coated titanium dioxide into the reactor and let it stand for 20-30min, and then sinter it at a constant temperature 20-30min, to obtain silicon-oxygen modified titanium dioxide, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10-15:1, the standing temperature is 50-70°C, and the temperature of the constant temperature sintering treatment is 120-150°C; a5, the silicon-oxygen modified titanium dioxide is placed in water and fully stirred, taken out and dried, and then placed in the middle section of the reactor, and aluminum isopropyl alcohol vapor is introduced and stood for 10-20min, and the doped silicon-oxygen modified titanium dioxide is obtained after rapid cooling, the concentration of the silicon-oxygen modified titanium dioxide in water is 100-300g / L, and the stirring speed is 200-300r / min, the standing temperature is 140-150°C; the volume proportion of the aluminum isopropoxide vapor in the standing atmosphere is 10-15%, and the temperature of the rapid cooling is 100-105°C; a6, placing the doped silicon-oxygen modified titanium dioxide in a reactor and standing for 20-30 minutes, followed by high-temperature sintering to obtain aluminum oxide-silicon-oxygen modified titanium dioxide, the atmosphere of the reactor being a mixed atmosphere of nitrogen and water vapor, with a volume ratio of nitrogen to water vapor in the mixed atmosphere of 10:1-2, the standing temperature being 90-100°C, the high-temperature sintering temperature being 800-1000°C, and the sintering time being 1-2 hours;. Step 2, the titanium dioxide is pretreated before use, and the pretreatment steps include: b1, adding alumina-silica modified titanium dioxide to ethanol and ultrasonically treating it for 20-30 minutes, filtering to obtain preliminarily washed alumina-silica modified titanium dioxide, the mass ratio of the alumina-silica modified titanium dioxide to ethanol is 2:2-3, the ultrasonic frequency of the ultrasonic treatment is 50-70kHz, and the temperature is 20-30°C; b2, adding alumina-silica modified titanium dioxide to ethanol aqueous solution and ultrasonically treating it for 20-30 minutes, filtering to obtain prefabricated alumina-silica modified titanium dioxide, the volume proportion of ethanol in the ethanol aqueous solution is 60-70%, and the concentration of the alumina-silica modified titanium dioxide in the ethanol aqueous solution is 40 -70g / L, the ultrasonic frequency of the ultrasonic treatment is 70-80kHz, and the temperature is 40-60℃; b3, adding the aluminum oxide-silicone modified titanium dioxide to an ethanol ether mixture and performing low-temperature ultrasonic treatment for 40-50min, filtering and washing with an ethanol ether mixture, and spray drying to obtain a clean aluminum oxide-silicone modified titanium dioxide, wherein the volume ratio of ethanol to ether in the ethanol ether mixture is 3:2-3, the concentration of the aluminum oxide-silicone modified titanium dioxide in the ethanol ether mixture is 40-70g / L, the ultrasonic frequency of the low-temperature ultrasonic treatment is 70-80kHz, and the temperature is 5-10℃; the spray drying temperature is 80-90℃, the spray volume is 10-20mL / min, and the spray area is 100cm 2 ; Step 3: adding sodium chloride to ethanol and stirring evenly to form a colloidal solution, then adding titanium dioxide and ultrasonically dispersing for 20-30 minutes to obtain a mixed colloidal solution; the concentration of sodium chloride in ethanol is 200-400 g / L, the stirring speed for uniform stirring is 300-500 r / min; the amount of titanium dioxide added is 50-70% of the mass of sodium chloride, the ultrasonic frequency of ultrasonic dispersion is 60-80 kHz, and the temperature is 20-30°C; Step 4, mixing ascorbic acid with an ethanol aqueous solution and ball milling for 10-20 minutes to obtain a slurry, then slowly adding the slurry to the mixed glue, and stirring the mixture at a constant temperature to obtain a prefabricated slurry; the mass ratio of ascorbic acid to ethanol aqueous solution is 5:1-2, and the volume proportion of ethanol in the ethanol aqueous solution is 93-95%, and the mixing is performed by mechanical stirring at 100-200r / min; the pressure of the ball milling treatment is 0.3-0.5MPa, and the temperature is 10-20°C; the addition rate of the slurry is 1-2g / min, and the amount of ascorbic acid added is 70-80% of the mass of titanium dioxide, the temperature of the constant temperature stirring reaction is 50-60°C, and the stirring speed is 200-300r / min; Step 5: Filter the prefabricated slurry to obtain a precipitate, then add it to an ethanol-water solution and rapidly stir it. After filtering, wash it repeatedly to obtain a white precipitate. Step 6: Place the white precipitate into a mixture of ethanol and ether and stir, then spray dry and deposit to obtain highly dispersible titanium dioxide.
2. The method for preparing highly dispersible titanium dioxide according to claim 1, wherein: The volume proportion of water in the ethanol aqueous solution in step 5 is 10-20%, the concentration of the precipitate in the ethanol aqueous solution is 100-200 g / L, the stirring speed of the rapid stirring is 2000-3000 r / min, the repeated washing uses ethanol aqueous solution, and the volume proportion of distilled water in the ethanol aqueous solution is 10-15%.
3. The method for preparing highly dispersible titanium dioxide according to claim 1, wherein: The volume ratio of ethanol to ether in the ethanol-ether mixture in step 6 is 3:1-2, and the stirring speed is 500-1000 r / min.
4. The method for preparing highly dispersible titanium dioxide according to claim 1, wherein: The spray drying in step 6 has a spray volume of 5-10 mL / min and a spray area of 200-300 cm 2 , the temperature is 80-90℃.
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