Method for preparing aqueous high-dispersion nano titanium dioxide

The method for preparing aqueous dispersion of nanometre titanium dioxide

technical field

[0001] The preparation method of the invention relates to a nano material, relates to a method for preparing aqueous dispersion of nanometre titanium dioxide in particular method.

background technology

[0002] The nanometre titanium dioxide by aspergillus wherein a particle size, greater than the surface area, magnet is stronger, photochemical catalysis of ultraviolet absorption ability is stronger, wherein the surface is greater; the heat conductivity of the is widely applied in solar battery, a gas purifying, the sewage treatment and cleaning material field. The synthesizing 1980s, the nanotechnology is introduced extracellular our textile, fieldThe 90's, positioning of national and research, projectUse of; the nanotechnology of extracellular our are in a way of ratio, wherein the nanometre titanium dioxide with the application prospect of the textile, industrial to with a and anti-aging, high-intensity solution, antistatic, antibacterial and so on, wherein of the textile new material, which is a sheet functions of ABR+OBR process in.

[0003] The preparation method of titanium dioxide a plurality literature, expressed use of the surface of the raw materials with purity of Zhihe the titanium tetrachloride. Purity of ester of the high purity of the raw material; and avoid introducing the foreign ion as far as material, to preparing the method for high requirement although, so as the purity is high, the particle size is small, coarse diameter is narrow nanometre powder, wherein the material is cost, high in drying and oil is easy to create the reunited of nanometre titanium dioxide intergranular. A purity of each, titanium tetrachloride, low-cost the process for is operator, more scientific researchers - using titanium tetrachloride of the raw material for nanometre titanium dioxide, to Guangshe Batch and so on TiCl4 and adding of the former of the ethanol, alcoholysis and drying, the powder titanium dioxide; Niederberger and Stucky realized by dropping TiCl4 to efficient intermediate the alcohol, a gel, a to the; the preparation of the grain size of 4-8nm with high within The anatase. A main question is further nanometre titanium dioxide is prepared from a run through the oil, which is easy to create the reunited of intergranular.

[0004] Nanometre TiO2 application of the textile the method has two generally. Method for mixing the nanometre powder 1102 as the polymer main body, spins the process to obtain the fibre is the melt; andThe method of light suitable for the chemical fibre, and spinning of the TiO2 particles, wherein of the reunited powder, the anti-blockage is formed and is formed behead, grinding loom of the questions, and particle is not are. The multimer TiO2 to the sheet is; the dispersing the water the drying refinement's finished product TiO2 powder, soaking process of single or an application of the sheet, or and preparation and recombinant of the TiO2 and so on,, Wherein the method is the TiO2 particle dispersion the preparation question, powder is uniformly distributed; and nanometre titanium dioxide from without said to the fibre, a hard to adhere fixed to the surface, wherein the rolling, the power of the physical absorption of the texture, wherein one or multiple, washing textile the lost photo-catalysis and. Recombinant wherein a coating, centigrade depends adhesive to adhere fixed to the texture, although fastness to the claim, wherein the medicine to the reducing, and as a result of the TiO2 particle of the covering adhesive, being with the external environment, the photo-catalysis activity is substantially therefore, TiO2 powder the application of textile comprising an inner limit.

The invention

[0005] Meshes of the invention is relates to a is easy to conduct the process for producing the obtained according to overcome the existing technology, comprising is a precipitating the method for preparing aqueous dispersion of nanometre titanium dioxide.

[0006] Meshes of the invention can the preaeration following technical solution is regulated:

[0007] A preparation preparing the aqueous dispersion of nanometre titanium dioxide the method, the is a characterised, comprising the following steps:

[0008] (1) Into the dispersing agent or surfactants deionized water, the concentration of dispersing agent or surfactant is 0 wt%. _12wt%, by dissolving stirring, the mixed solution;

[0009] (2) TiCl4 is added by dropping in the mixed solution, adding by dropping the method to conduct stirring and adding by dropping in a 20-60min, in the TiCl4 the complete; and comprises TiCl4 hydrolysate mixed solution;

[0010] (3) Is a TiClyK alpha-aluminium the mixed solution continuously stirring to 20-60min, before adding the deionized water; and wherein the heating rate is 3°C /min; the temperature is 30-60 -100°C, the insulating stirring, 2h_8h

[0011] (4) Cooling solution in the step (3) according to room temperature and standing curing 6h_14h, the nanometre titanium dioxide suspension for crystallizing the suspension liquid, filtering and deionized water washing and crystallizing in the nanometre titanium dioxide, adding deionized water to obtain the final product.

[0012] The step (1) the dispersing agent is an inorganic dispersing agent or the high - subclass dispersing agent, the inorganic an dispersing agent is comprising the sodium hexametaphosphate, high - subclass dispersing agent is a polyacrylamide, polyethylene glycol or polyvinylpyrrolidone.

[0013] The step (1) the surfactant is sodium dodecyl sulphate.

[0014] The step (2) TiCl4 and mixing solution volume ratio of 1: (2-5).

[0015] The step (3) the mixed solution of de-ionized water volume ratio of 1: (2-5).

[0016] The step (4) of the product is Contains concentration of _30 1-3 wt% TiO2 emulsion.

[0017] Compared to the existing technology, invention has the following: functional

[0018] A main of the:

[0019] (1) Is titanium tetrachloride raw material is the aqueous dispersion of titanium dioxide of the invention is preparation, low-cost, wherein the source of widespread, wherein it is low;

[0020] (2) Titanium dioxide according invention for preparing without high-temperature sintering can be to obtain the crystal and titanium dioxide, avoided the high-temperature to a crystalline phase change wherein the crystal grain according to grow for rapidly, so as the superfine nanometre titanium dioxide particles, the technique is simple, is ladder-shaped of the operation, wherein is easy to conduct the production process;

[0021] (3) In the aqueous dispersion of titanium dioxide emulsion the titanium dioxide concentration of high, the particle is sequentially; the particle size of less than 100 nm, wherein the is good, for a long time of depositing, wherein the no precipitate and acid is not converge the collecting to form the flock;

[0022] (4) Under the different reaction condition the obtained under the different titanium dioxide crystal, wherein the titanium dioxide crystal or anatase and rutile or anatase thereof.

Brief description of the drawings

[0023] With 1 of the heating IN-SITU of titanium dioxide the pharmaceutical composition according to claim 1, wherein

[0024] With 2 of the heating IN-SITU of titanium dioxide the pharmaceutical composition according to claim 2, wherein

[0025] With 3 to any ratio of the IN-SITU of heating Voltage.

detailed description of illustrated embodiments

[0026] Following steps of detail to the invention of light of the herein described and concrete compulsive.

[0027] Of 1 as

[0028] centigrade in the water - bath, wherein the Of one of the 30ml deionized water, by dissolving, fuels into a flask head, wherein the amount of TiCl4 catalyst is added by dropping in the flask, adding by dropping the method to conduct stirring, simultaneously controlling the dropping speed, removal of the hydrolysis reaction is thorough; A stirring min, then adding 105ml deionized water; A liquid-liquid to 50-60 degrees centigrade, the heating speed is 3°C /min; the temperature of the crystallizing point, centigrade under conditions crystallizing, 2hCooling to room temperature, the standing curing 12 hours and nanometre titanium dioxide suspension for crystallizing, filtering the suspension, the deionized water washing 2 times; of at Cl_ of nanometre titanium dioxide, adding a certain amount of the deionized water to 30% with concentration of the TiO2 solution. Figure 1 is the concentration of the heating IN-SITU of titanium dioxide 6% of kollidons. At the time of the crystal is of rutile-type, the average grain diameter of 68nm, the Voltage solution of the prepared, the standing wherein the present of of months.

[0029] Of 2 as

[0030] centigrade in the water - bath, and Mixture of sodium hexametaphosphate in the 30ml deionized water, by dissolving, fuels into a flask head, wherein TiCl4 catalyst is added by dropping in flask, adding by dropping the method to conduct stirring, simultaneously controlling the dropping speed, removal of the hydrolysis reaction is thorough; A stirring min, then adding 105ml deionized water; A liquid-liquid to 50-60 degrees centigrade, the heating speed is 3°C /min; the temperature of the crystallizing point, centigrade under conditions crystallizing, 2hCooling to room temperature, the standing curing 12 hours and nanometre titanium dioxide suspension for crystallizing, filtering the suspension, the deionized water washing 2 times; of at Cl_ of nanometre titanium dioxide, adding a certain amount of the deionized water to 30% with concentration of the TiO2 solution. Figure 2 is a concentration of 0. the heating IN-SITU of titanium dioxide 6% of sodium hexametaphosphate and. At the time of the crystal is the anatase, the average grain size ultraviolet absorbing, the Voltage solution of the prepared, the standing wherein the present of of months, wherein the is an aerobic.

[0031] To 1 and

[0032] centigrade in the water - bath, adding the catalyst is TiCl4 slow to the 30mL deionized water, stirring min, that is added to the 105mL deionized water, to the total volume of the solution is 150mL. A liquid-liquid to 50-60 degrees centigrade, the heating speed is 3°C /min, the temperature to crystallization degrees centigrade for 4 hours, cooling to room temperature, the standing curing 12 hours and nanometre titanium dioxide suspension for crystallizing, filtering the suspension, the deionized water washing 2 times; of the crystallizing in The nanometre titanium dioxide, adding a certain amount of the deionized water to 30% with concentration of the TiO2 solution.

[0033] To 2 and

[0034] centigrade in the water - 15mLTiCl4, adding by dropping slow to the 30mL deionized water, stirring min, that is added to the 105mL deionized water, to the total volume of the solution is 150mL. A liquid-liquid to 50-60 degrees centigrade, the heating speed is 3°C /min, the temperature to crystallization degrees centigrade for 4 hours, cooling to room temperature, the standing curing 12 hours and nanometre titanium dioxide suspension for crystallizing, filtering the suspension, the deionized water washing 2 times; of the crystallizing in The nanometre titanium dioxide, adding a certain amount of the deionized water to 30% with concentration of the TiO2 solution.

[0035] To 3 and

[0036] centigrade in the water - 15mLTiCl4, adding by dropping slow to the 30mL deionized water, stirring min, that is added to the 105mL deionized water, to the total volume of the solution is 150mL. A liquid-liquid to 50-60 degrees centigrade, the heating speed is 3°C /min, the temperature to crystallization degrees centigrade for 4 hours, cooling to room temperature, the standing curing 12 hours and nanometre titanium dioxide suspension for crystallizing, filtering the suspension, the deionized water washing 2 times; of the crystallizing in The nanometre titanium dioxide, adding a certain amount of the deionized water to 30% with concentration of the TiO2 solution.

[0037] Figure 3 is at each point is centigrade, 9 degrees CENTIGRADE, centigrade, and IN-SITU for heating the titanium weight to about. A and content of the crystallization, b is a crystalline, is between the crystallization. Compound obtained in degrees centigrade and under the crystallization is anatase or mixture of centigrade, the average grain diameter of 95nm, anatase-type the content of 38. 2%; a mean grain size is 81nm, anatase-type the content of 34. 3%; The degrees centigrade by rutile-type nanometre TiO2; the average grain diameter of 77nm. The centigrade, centigrade; the crystallization of the TiO2 solution is 4 hours prepared settles, or more days after of the following and.

[0038] Of 3 as

[0039] The method for preparing aqueous dispersion of nanometre titanium dioxide, comprising the following steps:

[0040] (1) Into the polyacrylamide the de-ionized water, the polyacrylamide is 0 wt%., by dissolving stirring, the mixed solution;

[0041] (2) TiCl4 is added by dropping in the mixed solution, TiCl4 and mixing the aqueous solution volume ratio of 1: 2nd, Adding by dropping the method to conduct stirring and adding by dropping in a min; in the TiCl4 the complete; and comprises TiCl4 hydrolysate mixed solution;

[0042] (3) Is a TiCl4 hydrolysate's mixed solution is continuously stirring min, before adding the de-ionized water, the mixed solution of de-ionized water volume ratio of 1: 2nd, And wherein the heating rate de-waxing is; the temperature to 60°C°C, the insulating at 6-8 hours;

[0043] (4) Cooling solution in the step (3) according to room temperature and standing and curing, obtaining the nanometre titanium dioxide suspension of crystallization, of crystals of the nanometre titanium dioxide the suspension filter and deionized water, the final adding deionized water to obtain the product, wherein the concentration is 10 percent by weight of TiO2 emulsion.

[0044] Of 4 as

[0045] The method for preparing aqueous dispersion of nanometre titanium dioxide, comprising the following steps:

[0046] (1) Is the sodium dodecyl sulfate the de-ionized water, the sodium dodecyl sulfate the concentration of 12wt%, by dissolving stirring, the mixed solution;

[0047] (2) TiCl4 is added by dropping in the mixed solution, TiCl4 and mixing the aqueous solution volume ratio of 1: 5th, Adding by dropping the method to conduct stirring and adding by dropping in a 60min, in the TiCl4 the complete; and comprises TiCl4 hydrolysate mixed solution;

[0048] (3) Is a TiCl4 hydrolysate's mixed solution continuously stirring to 60min, before adding the de-ionized water, the mixed solution of de-ionized water volume ratio of 1: 5th, And wherein the heating rate de-waxing is; the temperature is 50-100 degrees centigrade, the insulating stirring, 2h

[0049] (4) Cooling solution in the step (3) according to room temperature and standing curing 14h, the nanometre titanium dioxide suspension of crystallization, of crystals of the nanometre titanium dioxide the suspension filter and deionized water, the final adding deionized water to obtain the product, wherein the concentration is 30 percent by weight of TiO2 emulsion.