Process for preparing rutile-phase nano-titanium dioxide

A rutile the preparation method for nanometre titanium dioxide

technical field

The invention relates to any one or the preparation method for nanometre titanium dioxide, and independently of relates to a nano oxide in the low-temperature the method thereof, belonging to the non-metallic inorganic nano the technical field.

background technology

The titanium dioxide with, or anatase titanium dioxide and titanium plate 3 of crystal structure in the quality; the thermostability oxide is preferably, the natural brookite to 650℃ more of the oxide, anatase-type of the conditions of 915℃ as rutile, wherein of the claims, irreversible. The or atom device of titanium dioxide is compact, the relative density of the r.i of the quite, having high and a beam, and has good environment-friendly capability to the radiation of ultraviolet. The rutile-type titanium dioxide - comprising the step of hiding power and tinting, strength of the white on the modern industry. Wherein the rutile-type titanium dioxide particle is less than a micron, dimension to photo-catalysis ability of the physical properties is an evolutionarily significant reinforced, wherein the production and under a widespread application thereof.

The system for the titanium dioxide, for use a) expensive titanium organic salt (such as follows: The isopropanol titanium, purity of ester) and so on an precursor, wherein titanium tetrachloride and titanium sulphate and so on does not happen the organic salt titanium. The technique for preparing method mainly comprising: A, by hydrothermal method of metallic materials method. Use of the different, wherein the powder is carried out at room temperature to chamber is non-final component, obtainable the type of the calcined, the temperature higher thermal (is higher than 900℃ generally), obtainable by rutile. A is - oil, crystal grain and fast, being obtained by the particle is wherein the nano-scale rutile-type titanium dioxide powder. By the seeks, wherein the low temperature for preparing nanometre the method of rutile-type titanium dioxide is the hot investigates researching the field. Zilong Tang and having a [Zilong Tanget a7., And A Physical and 77(2002) 314-317 into the one as purity of ester of Ti (OC4H9) 4] as raw material, wherein 40-50℃ by the method of hydrochloric acid and nano-scale rutile-type titanium dioxide; Zhang Qinghong and others of more of invention, application of: 99113693.4 Into the one as titanium tetrachloride as raw material, wherein the medicinal composite is titanium tetrachloride the speed, comprising the nano-scale rutile-type titanium dioxide under room temperature the method.

The invention

Question weight of the invention is solve to provide a method for preparing the nano oxide in the low-temperature the method thereof.

The invention claims a technical solution according to weight of question solution is a titanium tetrachloride and organic additive: The agar, polyvinyl alcohol, carboxymethyl cellulose or the combination of the raw material, wherein the titanium tetrachloride having the presence of organic additive, wherein precipitating the centrifugal separation, the washing, drying, wherein the low temperature 200-400℃ to processing process, a wherein the rutile-type nanometre titanium dioxide.

Presently the methane detail invention technical solution.

Method for preparing the nano oxide in the low-temperature the method thereof, the is characterised in water, in step: The first step raw materials raw material is titanium tetrachloride and organic additive: , Of polyvinyl alcohol, carboxymethyl cellulose sodium or polyethylene,The preparation of the second reaction solution is ml of distilled water in the reactor, weighing the 0.5g organic additive, then adding into distilled water, under room temperature for stirring uniformly; Sanbushui Fan In the used for water - bath cooling distilled water and organic additive mixed solution, wherein the cooling process is added that wherein the added by dropping titanium tetrachloride 10ml to the mixed solution, the mixed solution the temperature of 10℃, wherein the solution a, to that are stirred for 5-20 min, the mixed solution the temperature to 90-95℃, titanium tetrachloride hydrolysis, in the pulpous; andThe fourth the separation, washing and drying pulpous of cooling the third step according to the room temperature; and precipitating the centrifugal separation, the washing, drying 80-120℃, in the gas iron powder; The gas iron powder is the fifth step to the step are obtained by 200-400℃ the oil, average grain size weight of the whose rutile-type nanometre titanium dioxide powder.

The third in the hydrolyzing process of titanium tetrachloride is a complex the reaction process, wherein the chemical formula of the represented as follows: TiCl4+2H2O=TiO2+4H++4Cl-

Compared to the background technology, invention has the following beneficial and: 1st, The method of the invention is a oxide in the low-temperature the titanium dioxide, wherein of the or the production cost of titanium dioxide.

2nd, A reaction at low temperature, which is easy to obtain the nanometre magnitude rutile-type titanium dioxide.

3rd, And the adding the anion additive, preparing the or the particle of method, wherein the organic additive method of easily obtained by removing method of thermal decomposing.

4th, And organic group titanium salt (such as follows: The isopropanol titanium, purity of ester) is the preparation method of raw material, diluting the method of the invention is easily and a, the raw material is the method of the invention is used easier much.

Brief description of the drawings

With 1 of the sample X-ray diffraction light (XRD in figure according to the invention preparation method.

With 2 of the sample field of into the electron microscope following according to the invention preparation method.

detailed description of illustrated embodiments

All of examples and concrete in the operation of the preparation method.

The substantially as adding 1 ml of distilled water in the reactor, weighing the 0.5g agar, then adding into distilled water, under room temperature for stirring uniformly. A ice water - bath cooling distilled water and of mixed solution, wherein the cooling process for is. A stirring added by dropping the 10ml titanium tetrachloride to the mixed solution, the mixed solution the temperature of 10℃. The solution a, to that are stirred for 5-20 min. The mixed solution the temperature to 90-95℃, titanium tetrachloride hydrolysis, in the pulpous and. Pulpous of cooling the room temperature; and precipitating the centrifugal separation, the washing, drying 80-120℃, in the gas iron powder, wherein the 400℃ of the calcined, the average grain diameter of the nanometre sio2 rutile-type titanium dioxide.

The substantially as adding 2 ml of distilled water in the reactor, weighing the 0.5g polyethylene, then adding into distilled water, under room temperature for stirring uniformly. A ice water - bath cooling distilled water and polyethylene mixed solution, wherein the cooling process for is. A stirring added by dropping the 10ml titanium tetrachloride to the mixed solution, the mixed solution the temperature of 10℃. The solution a, to that are stirred for 5-20 min. The temperature to 90-95℃, titanium tetrachloride hydrolysis, in the pulpous and. Pulpous of cooling the room temperature; and precipitating the centrifugal separation, the washing, drying 80-120℃, in the gas iron powder, wherein the 300℃ of the calcined, the average grain size of the 25nm rutile-type nanometre titanium dioxide.

The substantially as adding 3 ml of distilled water in the reactor, weighing the 0.5g polyvinyl alcohol, then adding into distilled water, under room temperature for stirring uniformly. A ice water - bath cooling distilled water and polyvinyl alcohol mixed solution, wherein the cooling process for is. A stirring added by dropping the 10ml titanium tetrachloride to the mixed solution, the mixed solution the temperature of 10℃. The solution a, to that are stirred for 5-20 min. The mixed solution the temperature to about 90-95℃, titanium tetrachloride hydrolysis, in the pulpous and. Pulpous of cooling the room temperature; and precipitating the centrifugal separation, the washing, drying 80-120℃, the gas iron powder, wherein the 300℃ of the calcined, the average grain size of the 25nm rutile-type nanometre titanium dioxide.

The substantially as adding 4 ml of distilled water in the reactor, weighing 0.5g carboxymethyl cellulose Nagat according to the distilled water, under room temperature for stirring uniformly. A ice water - bath cooling distilled water and carboxymethyl cellulose sodium's mixed solution, wherein the cooling process for is. A stirring added by dropping the 10ml titanium tetrachloride to the mixed solution, the mixed solution the temperature of 10℃. The solution a, to that are stirred for 5-20 min. The temperature to 90-95℃, titanium tetrachloride hydrolysis, in the pulpous and. Pulpous of cooling the room temperature; and precipitating the centrifugal separation, the washing, drying 80-120℃, in the gas iron powder, wherein the 200℃ of the calcined, the average grain size is deposited up the rutile-type nanometre titanium dioxide.