Preparation method of controllable-phase-change titanium dioxide nano-particles

The preparation method of phase-transformation controllable nano particle

technical field

[0001] The invention relates to the preparation method of nano particle, specifically the preparation method of relating to the phase-transformation controllable nano particle.

background technology

[0002] Titanium dioxide and a industrial auxiliary material, to the wide, and wherein type crystal phase and rutile crystalline phase of a compound of structure, comprising an inner difference in the condensation.

[0003]Use of a, the purity method of nano-level titanium dioxide is multiple, a synthesis method of the template method, wherein the wet process, the splashing method, anodic oxidation of ABR+OBR process in. A, mixing researching systematization of titanium dioxide or phase-transformation controllable titanium dioxide. A EG82013 and 30% part rutiles organic poison and preferably of titanium dioxide nanometre smoothing catalytically the power of 70% anatases, and other performance, catalytically to H2S gas, or content of the maximum. Use of additive existence's the catalyst is the gas preparation method does not happen thorough the discussion of the nano-scale and anatase titanium oxide, along with the constant composed of gas industry, titanium dioxide ACCLIMATION CHANNEL and R is the content with controllable is a hot of for future further.

[0004] The although of titanium dioxide with preparing performed by mass, research to claim CN201210177244.8, CN201210161461.8, CN201110052773.0 and CN201110437804.4, wherein a preparation method and control reacts according to publicizes, wherein a process complicated a hard the industrial production, wherein the phase-transformation is controllable unimaginable. Therefore prior art is not capable disposable groove with according to the mixed product, comprising adding a difficulty to the industrial in.

The invention

[0005] How invention wants the solve the weight problems to overcome prior art the deletion, the method of any one phase-transformation controllable nano particle.

[0006] A solve the weight problems; the preparation method of the phase-transformation 'controllable nano particle comprising the following steps:

[0007] I) hydrolysis is conducted:

[0008] The above the following ice salt bath, I ) is a ml of titanium oxide of rapid 1-1OOOmL of de-ionized water, stirring to obtain a white sediment mixed liquid.

[0009] 2)sol/gel react:

[0010] In step I) and mixing liquid of the ammonium sulphate solution by adding dropwise, wherein the white sediment in the mixed liquid, by uniformly solution, heating to 30 degrees centigrade for heating the solution I to 10 hours, wherein the evaporated liquid slow, the form sol/gel, cooling to room temperature, and adjusting the cooling process PH to 6.0-9.0.

[0011] 3)Filter: washing

[0012] The step 2) is sol/gel decompressing extracting, filtering, the de-ionized water washed repeatedly to the non-porous and ion, adding the dried grinding, the metastable of system.

[0013] 4)High-temperature sintering:

[0014] The step 3) is precursor compound and salt the root 1_24 the 300-800°C under the condition, the removing impurity, comprising the phase-transformation controllable nano particle.

[0015] A preferably, wherein the ice bath for intermediate preferably from the ice and NaCl, KCL, Na2S04 and K2504 one or the combination of multiple.

[0016] A preferably, the composite salt is preferably Of NaCl and according to composite salt thereof according to a certain ratio of stirring.

[0017] A preferably wherein the titanium oxide the volume is preferably ml, wherein the de-ionized water is preferably is 500mL, said composite salt preferably Of NaCl and according to 1:1, stirring the step I) a ice salt temperature preferably, claims step 3) heating temperature preferably centigrade, heating time preferably 10 hours.

[0018] Beneficial action of the invention is:

[0019] 1st, Wherein the process of the controllable the nanometre ball titanium dioxide, phase-transformation

[0020] 2nd, Wherein the process is applied nanometre titanium dioxide ball for the preparation of discharging the industrial preparation,

[0021] 3, Wherein the process comprises a halogen extent growth of nanometre titanium dioxide application of;

[0022] 4th, For preparing process is ladder-shaped for processing.

[0023] The preparation method of the invention phase-transformation controllable nanoparticle, the technical device is simple, technique of cleaning; the light energy the nanometre ball titanium dioxide phase-transformation is controllable, the ratio of of high-precision control crystal form titanium dioxide, 1-50% is suitable for the industrial auxiliary material is wherein the content of stricter achieves nanoparticle preparation.

brief description fo the drawings

[0024] Of to the invention phase-transformation controllable nanoparticle in a further explanation the method for figure's are preparation method:

[0025] With 1 of the IN-SITU of heating for nanometre titanium dioxide of the phase-transformation controllable nanoparticle preparation method dissimilar wherein the preparation, discharging

[0026] With 2 of the phase-transformation controllable nanoparticle method for preparing anatase content rate of the roasting time relational pattern.

Specifically embodiment

[0027] Embodiment of: The preparation method of the phase-transformation controllable nano particle comprising:

[0028] I) hydrolysis is conducted:

[0029] Of claims the ice bath salt, the fed titanium oxide quickly of 1-10 of de-ionized water, stirring to obtain white sediment mixed liquid;

[0030] 2)sol/gel react:

[0031] In step I) and mixing liquid of the ammonium sulphate solution by adding dropwise, wherein the white sediment in the mixed liquid, by uniformly solution, heating to for heating the solution I hours, wherein the evaporated liquid slow, the form sol/gel, cooling to room temperature, and adjusting the cooling process IS 6.0 to.

[0032] 3)Filter: washing

[0033] The step 2) is sol/gel decompressing extracting, filtering, the de-ionized water washed repeatedly to the non-porous and ion, adding the dried grinding, the metastable of system.

[0034] 4)High-temperature sintering:

[0035] The step 3) is precursor and KCl and NaCl roasting is 24 degrees centigrade under the condition according to 1:1 mixing's composite salt, the removing impurity, comprising the phase-transformation controllable nano particle.

[0036] Embodiment of: The preparation method of the phase-transformation controllable nano particle comprising:

[0037] I) hydrolysis is conducted:

[0038] minutes in the ice bath salt, the ml titanium oxide of rapid 500mL of de-ionized water, stirring to obtain white sediment mixed liquid.

[0039] 2)sol/gel react:

[0040] In step I) and mixing liquid of the ammonium sulphate solution by adding dropwise, wherein the white sediment in the mixed liquid, by uniformly solution, heating to the temperature for heating the solution 5, wherein the evaporated liquid slow, the form sol/gel, cooling to room temperature, and adjusting the cooling process IS 8 to.

[0041] 3)Filter: washing

[0042] The step 2) is sol/gel decompressing extracting, filtering, the de-ionized water washed repeatedly to the non-porous and ion, adding the dried grinding, the metastable of system.

[0043] 4)High-temperature sintering:

[0044] The step 3) is precursor and KCl and NaCl roasting is 12 degrees centigrade under the condition according to 1:1 mixing's composite salt, the removing impurity, comprising the phase-transformation controllable nano particle.

[0045] An embodiment: The preparation method of the phase-transformation controllable nano particle comprising:

[0046] I) hydrolysis is conducted:

[0047] Of claims the ice bath salt, the ml of titanium oxide of rapid IOOOmL of de-ionized water, stirring to obtain white sediment mixed liquid;

[0048] 2)sol/gel react:

[0049] In step I) and mixing liquid of the ammonium sulphate solution by adding dropwise, wherein the white sediment in the mixed liquid, by uniformly solution, heating to 8 degrees centigrade for heating the solution 10, wherein the evaporated liquid slow, the form sol/gel, cooling to room temperature, and adjusting the cooling process IS 9 to.

[0050] 3)Filter: washing

[0051] The step 2) is sol/gel decompressing extracting, filtering, the de-ionized water washed repeatedly to the non-porous and ion, adding the dried grinding, the metastable of system.

[0052] 4)High-temperature sintering:

[0053] The step 3) is precursor and KCl and NaCl roasting is 24 degrees centigrade under the condition according to 1:1 mixing's composite salt, the removing impurity, comprising the phase-transformation controllable nano particle.

[0054] Wherein the pkctheta I, and discharging the precursor according to any embodiment preparation, a composite salt in a ratio is good, wherein centigrade is performed by roasting time, the roasting time is 2, 4, 6 and 8, 1-10, product for preparing discharging is titanium dioxide nanometre ball, the particle uniformly, the diameter is about 10 to deposited up. A heating 1 is WHEREIN the analysis is 2a of the obtained product, wherein the data by heating the counting performed under varying baking time titanium dioxide anatase is the total product, wherein the proportion by heating further can according into the product with two of anatase titanium dioxide and rutile-type titanium dioxide.

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[0057] Under the different I and anatase titanium dioxide mass fraction

[0058] Figure 1 and 2 shown as; and formula I am mounted to 2 in a form, and seen in Figure 2, discovered in the anatase in the mass ratio of the roasting time of the relationship linear. The improved by the roasting time, wherein the anatase and content of rutile-type, wherein according to the needed by a series of different content nanometre Tio2 particle, a root 19.31h according to the fitted time appropriately, the purity oxide, and from 2 to 19.3h the obtained two ends of the anatase and or different and phase, wherein the flow content to compared to the roasting time of counting, which has a wherein the control time, and easy to obtain.

[0059] The embodiment of a purpose of explaining of examples of the invention is used in the field professionals is carried out or use, wherein revise is to further the professionals in the field of the embodiment, therefore invention comprises, and is not limit of the embodiment, contains one of water or a water is describe, wherein the method, a method for and a product and novel and creative contains of the invention is publicize, wherein the into the invention in the extent of protection.