Method for preparing mixed crystal type titanium dioxide nano-powder and product thereof

A preparation method of the product for preparing the crystal nano-powder

technical field

[0001] The invention belongs to photo-catalysis material technical field, specifically, wherein relating to the or the anatase for the preparation of rutile-type the method and product of the crystal nano-powder.

background technology

[0002] A Voltage with the oxidization and a step, the is thorough process, the second and bottom of the stability is good, costs the advantages ore, comprising the wide one of photocatalyst according in recent years 40, wherein the composition is applied photolysis the water and carbon nitrogen is fixed with wide, wherein degenerating organic substance of the photo-catalysis aspects. The TiO2 photo-catalysis activity and crystalline form, within thereof, and grain size is sealed. TiO2 comprising a anatase, oxide and brookite the seed crystal structure, the research compound that and anatase or TiO2 a photo-catalysis activity, further - comprising the steps of anatase or) and TiO2 a height photo-catalysis performance. , Wherein the reality to seek is one or more is able to detect the preparation of the TiO2 correspondingly process of the simple process and low cost and way of the is controlled by mass.

[0003]Use of of a preparation method of the crystal is titanium dioxide is which uses the solating of gel method, the hydrothermal method or a micro-emulsion method. The preparation method is 1*10 to the power of comprises a type controlled by calcining heat or and said ion and TiO2 or mixed crystal product, existing the preparation methods' flaws elevating: (I), complicated is hard to the high-precision the control of the technical conditions, desired product obtained by wherein the height; (2) Stintering treatment process in the special device stintering, and reacting time-consuming growth, efficiency of the height, and a suitable for large batch the requirement; (3) Is of the compressing and ion is controls the process, regardless being of the addition or the adding time of high-precision a control. costs height, and water inlet is unavoidable impurities, is affecting the final product by. Therefore, present in the field of the crystal is titanium dioxide powder and preparation process further improve technique requirement. Present in the photo-catalysis material field to the crystal of titanium dioxide preparation process further improve technique requirement.

The invention

[0004] The process of the deletion and technique requirement of prior art, the aim of the invention is any one or the anatase for the preparation of rutile-type the method and product of the crystal nano-powder, wherein it is carried out the researches and improve the main reaction and reaction condition and other aspects, wherein the method is simple, low-density costs the nano-scale product, and is ladder-shaped is controlled in a suitable for large volume; the productionA mixed nano-powder crystal grain size of the resulting is small, the granularity uniformly; and an anatase and or two of structures, and displays the excellent photo-catalysis the capacity.

[0005] The process according to this invention claims surface, wherein any one of comprises a type for the preparation of rutile-type the method for crystal is nano-powder, the is a characterised, comprising the following steps:

[0006] a) is 22-57 the tetrabutyl titanate ester or isopropanol titanium of the de-ionized water to form the white sediment, separating white sediment and washing cleanly, and alcohol to the de-ionized water, and of a stirring in a further aspect dropwise the concentration is 40% to 3% acidic nitric acid, sulphuric wherein the stirring, the prepared in the transparent the titanium salt solution;

[0007] (b) is made of titanium salt solution is made of added as the reducing agent and fuel which is formed by the mixed solution, and urea with the titanium salt solution mol ratio of the titanium ions is 0. 4-4. 0;

[0008] (C) the high-temperature furnace is carried out in the step (b) a forming mixed solution is arranged in the -600°C centigrade self-propagating combustion, wherein from the obtained solution comprising a anatase and or two of structure of single crystal nanopowders.

[0009] A preceding claim, wherein the portion of the first tetrabutyl titanate ester or isopropanol titanium conducted with an sediment, wherein the sediment in the form of nitrate the nitric acid, the nitrate directly using the oxidant, filtering by oxidation reduction reaction can be with the reducing agent directly which has a titanium dioxide product, freezing temperature stintering treatment, simple operation,A further aspect, wherein the reaction is the self-propagating combined combustion sequence of quick, the whole combined sequence short time, mixture of several min, the beneficial for reducing integral production cost, comprising The Guangpin by the controllability.

[0010] A further preferably, wherein step (b), the urea and titanium salt solution mol ratio of the titanium ions is 0. 45-2. 5.

[0011] The are used as an fuel the synthesis according, following raw materials by weight, PH value, ignition temperature of the is a reaction process of the mass of the material. A and titanium salt solution the mol ratio of the titanium comprising the further used as thereof is in the range, wherein with multiple comparative the trials: The furnish material with a can be guaranteed the mixed solution self-propagating combustion, and obtaining the grain size is small, and uniformly nano-scale product, and wherein the integral mass is good.

[0012] A further preferably, wherein in the step (C), wherein the is used as the fuel, wherein of self-propagating combustion the ignition temperature is 1-10 about.

[0013] A further preferably, wherein step (b), further use of the glycine or citric acid to the urea, and which is a titanium salt solution mol ratio of the titanium ions is 0. Hours. 5.

[0014] Adjusting the glycine or citric acid the second used as the organic fuel, can be guaranteed wherein the organic reducing fuel is fully amount of the mixed solution, and at mixed solution of of reducing process or the reducing agent role. The suspension, wherein the glycine or citric acid and organic fuel the synthesis according, wherein with multiple comparative the trials obtained by and titanium an wherein the mol ratio of the organic thereof is in the range, wherein furnish material with a can be guaranteed the mixed solution self-propagating combustion, and wherein the mass is good.

[0015] A further preferably, wherein step (b), wherein in the titanium salt solution is added to the fuel in the process of the magnetic stirring.

[0016] A further preferably, wherein in the step (C), when using the or citric acid as fuel, is carried out to self-propagating combustion the ignition temperature is centigrade about.

[0017] According to the invention, and other, further - comprising any said crystal is nano-powder product.

[0018] A further preferably, the crystal is nano-powder with a grain diameter average diameter of about 15nm_150nm.

[0019] , Chamber according to the invention comprises the anatase for the preparation of the oxide of the same and product of the prior art crystal is nano-powder, mainly comprising the steps of: advantages

[0020] I, wherein the reaction condition to preparing the crystal titanium dioxide powder of the main agent and other aspects of the improve, the can not be comprises increasing yield efficiency, and control of amplification product, inThe suspension, self-propagating a combustion and stintering processing device has a speed is quicker, and to avoid the ion and inlet, the energy crosslinked and sustained-release the costs, therefore suitable for mass production slag, especially

[0021] 2nd, Wherein the following raw materials by weight of ignition temperature to claims an organic fuel the formula of the conditions, further can be guaranteed mixed solution self-propagating combustion the reaction rate at the same time improve the synthetic fully system, and has good of nanometre powder;

[0022] 3rd, Wherein the crystal is nano-powder the grain size of the resulting in a small according to the invention, the granularity uniformly, wherein the grain size average diameter of about 15nm-150nm; and an anatase and or two of structures, and displays the excellent photo-catalysis the capacity.

brief description fo the drawings

[0023] The heating I am polyester to the invention claims a heating for preparing the crystal, nano-powder

[0024] Figure 2) of the sample preparation SEM heating according to the invention embodiment of the;

[0025] Figure 3 according to the invention 2 embodiment the 2# sample SEM heating according to result in;

[0026] Figure 4 according to the invention 3 embodiment the 3# sample SEM heating according to result in;

[0027] Figure 5 according to the invention embodiment 4 4# the sample SEM heating according to result in;

[0028] Figure 6 to any 1#_4# performing sample test forming IN-SITU, pattern

[0029] With 7 of the methyl orange solution and performing to any 1#_4# the sample degenerating of drawing schematic.

Specifically embodiment

[0030] With an inkjet ink, technical solution of the advantages the invention even more clearly understands by the following with a herein described with the embodiment, wherein the invention further detail in explained. The area, the embodiment of specifically display process to explain invention, is only not used for treating the invention. Moreover, the technological feature of the invention each embodiment of claims the invention refers to a number wanted the consists of conflict to any of the inter-combination.

[0031] Heating I according to the invention comprises the anatase titanium oxide and flow of heating the crystal nano-powder. A evaluating shown as solution, comprising a type for the preparation of the or two of structure of single crystal nanopowders, firstly, the weighing the ingredients tetrabutyl titanate ester or isopropanol titanium added to the is added in the de-ionized water solvent, and forming white sediment; Use of the de-ionized water washing is cleaned by the white sediment separation, and alcohol on of a stirring in a further aspect dropwise condensation added to the de-ionized water is 40% to 3% acidic nitric acid, sulphuric wherein the stirring, the prepared in the transparent the titanium salt solution.

[0032] , And is made of titanium salt solution of sodium, weighed the ingredients with urea (further can be used in or citric acid second), and a to the titanium salt solution which is carried out the magnetic stirring is a forming mixed solution, when works as and urea, wherein a titanium salt solution the mol ratio of titanium ions is 0. 4-4. 0 Acrylate, preferably is 0. 45-2. 5; A when adding the decays or 1 檬 the acid, comprising a titanium salt solution the mol ratio of titanium ions is 0. Hours. 5. The action of urea or similar material is as follows self-propagating combustion synthesis's organic fuel, and also taking the oxidation and reducing agent in the reduction reaction system.

[0033] , Wherein the step of forming mixed solution of the centigrade -600°C the high-temperature furnace in the consists of the polymer system, and is carried out self-propagating combustion by the organic; fuelIgnites degrees centigrade under the condition, the mixed solution self-propagating combustion, the obtained solution comprising a type from of the or two of structure of single crystal nanopowders.

[0034] Wherein after the method for manufacturing the grain size of the crystal nano-powder product resulting is 15nm_150nm.

[0035] A embodiment

[0036] Weighing 10. of the tetrabutyl titanate ester, adding proper de-ionized water of the tetrabutyl titanate ester complete conducted obtain white sediment, separating white sediment is cleaning wherein washing with de-ionized water, and then adding 30mL de-ionized water is sediment; of a stirring in a further aspect to about slowly adding of concentrated nitric acid, fully stirring wherein the sediment completely dissolved, obtaining clear transparent solution; The added weight of the solution is controlled to 0. 72g-7. the polyurethaneurea with the polymer and de-ionized water of the embodiment, thereof is 0. Slg urea and proper de-ionized water), the magnetic stirring, by clarifying ml of transparent mixed solution; The mixed solution is arranged in the 350°C high-temperature furnace, the solution after the evaporating and boiling and bubbles, wherein the combustion fierce reaction, wherein the combustion a reaction, the obtained fluffy a powder. The is made the grinding powder, obtain the sample preparation.

[0037] Figure 2) of the sample preparation SEM heating according to the invention embodiment, as described, 1# sample particle size distribution uniformly; the particle size of less, average particle diameter of about 15nm.

[0038] embodiment 2

[0039] Weighing 8. 53g the isopropanol titanium, adding proper de-ionized water and isopropyl alcohol titanium rod conducted obtain white sediment, separating white sediment is cleaning wherein washing with de-ionized water, and then adding 30mL de-ionized water is sediment; of a stirring in a further aspect to about slowly adding of concentrated nitric acid, fully stirring wherein the sediment completely dissolved, obtaining clear transparent solution; The added weight of the solution is controlled to 0. 72g-7. the polyurethaneurea with the polymer and de-ionized water of the embodiment, thereof is 4 g. urea and proper de-ionized water), the magnetic stirring, by clarifying ml of transparent mixed solution; The mixed solution comprising at the temperature high-temperature furnace, the solution after the evaporating and boiling and bubbles, wherein the combustion fierce reaction, wherein the combustion a reaction, the obtained fluffy a powder. The is made the grinding powder, obtain the 2# sample.

[0040] Figure 3 according to the invention 2 embodiment the 2# sample SEM heating according to result, FORMULA, the 2# sample particle size distribution uniformly; the particle size of less, average particle diameter of about 25nm.

[0041] embodiment 3

[0042] Weighing 10. with the tetrabutyl titanate ester, adding proper de-ionized water of the tetrabutyl titanate ester complete conducted obtain white sediment, separating white sediment is cleaning wherein washing with de-ionized water, and then adding 30mL de-ionized water is sediment; of a stirring in a further aspect to about slowly adding of concentrated nitric acid, fully stirring wherein the sediment completely dissolved, obtaining clear transparent solution; The added weight to control the solution I. 13g-3. 38g the glycine and proper in the de-ionized water (thereof is 2 to the embodiment g. glycine and proper de-ionized water), the magnetic stirring, by clarifying ml of transparent mixed solution; The mixed solution is centigrade for high-temperature furnace, the solution after the evaporating and boiling and bubbles, wherein the combustion fierce reaction, wherein the combustion a reaction, the obtained fluffy a powder. The is made the grinding powder, obtain the 3# sample.

[0043] Figure 4 according to the invention 3 embodiment the 3# sample SEM heating according to result, FORMULA, 1# sample particle size distribution uniformly; the particle size of less, average particle diameter of the thick.

[0044] embodiment 4

[0045] Weighing 8. 53g the isopropanol titanium, adding proper de-ionized water and isopropyl alcohol titanium rod conducted obtain white sediment, separating white sediment is cleaning wherein washing with de-ionized water, and then adding 30mL de-ionized water is sediment; of a stirring in a further aspect to about slowly adding of concentrated nitric acid, fully stirring wherein the sediment completely dissolved, obtaining clear transparent solution; The added weight of the solution is controlled to 3. 15g-9. 46g citric acid and proper de-ionized water (of the embodiment thereof is 3. 78g citric acid and proper de-ionized water), the magnetic stirring, by clarifying ml of transparent mixed solution; The mixed solution is centigrade for high-temperature furnace, the solution after the evaporating and boiling and bubbles, wherein the combustion fierce reaction, wherein the combustion a reaction, the obtained fluffy a powder. The is made the grinding powder, obtain the sample 4#.

[0046] Figure 5 according to the invention embodiment 4 4# the sample SEM heating according to result, FORMULA, 4# sample particle size distribution uniformly, average particle diameter of about nm.

[0047] The is carried out the IN-SITU test direction facing the 1#_4# sample according to prepared from. Figure 6 to any 1#_4# performing sample test IN-SITU forming's pattern, into a preparation of 2# and control of XRD, wherein the used amount youth, synthetic TiO2 all of the anatase, along with the urea and content, wherein the powder of the compound type and oxide,3# And the 4# sample is a glycine and citric acid and organic fuel, wherein the synthesis of the anatase and oxide of rutile-type TiO2 powder.

[0048] An application of the 1#-4# d the sample 10mg/L ml of methyl orange solution of; the hidden the stirring minutes achiefs with an equilibrium, wherein the 50W high pressure mercury lamp is the light source, the liquid surface of the ultraviolet lamp distance is 25cm, and a controlling the temperature of the magnetic force the step of stirring and water - bath of about 293K. The illumination hours after using a sample, wherein the centrifugal separation, and clarifying solution is discharging, wherein the UV-2550 UV spectrophotometer measured using clear liquid the extinction, the degenerating efficiency of counting catalyst. With 7 of the methyl orange solution and performing to any 1#_4# the sample degenerating rate schematic drawing, such as picture seven is shown as, preparation and 2# sample photochemical catalysis of the height, methyl orange solution into the additive is the ultraviolet ray and rate is 80. 1% and 70 1%. .

[0049] The technical field reconstituted with human easy understood according to the mixture of the invention claims an embodiment, does not need to limit to the invention, each of any revises and equates the second and improve of the alcohol and position of the invention is so on, which comprises the invention extent of protection.