CN1478725A - Preparation method of crystal phase controllable titanium dioxide nanometer crystal - Google Patents
Preparation method of crystal phase controllable titanium dioxide nanometer crystal Download PDFInfo
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Abstract
A process for preparing the crystal phase controllable TiO2 nanocrystals includes such steps as hydrolyzing the Ti-cotnained compound in the aqueous solution of alcohol to obtain amorphous TiO2 powder, adding inorganic acid, hydrothermal treating, filtering, washing and drying. Its resultant TiO2 nanocrystal has the continuously regulatable ratio of anatase phase to rutile phase.
Description
Technical field
The present invention is a kind of anatase octahedrite and rutile method of the continuously adjustable nano titanium oxide of ratio mutually for preparing.Utilize present method not need high-temperature roasting just can obtain mixing the titanium dioxide nanocrystalline of crystalline phase, and the ratio of two kinds of crystalline phases can be by the continuous modulation of control preparation condition.
Background technology
Owing to have excellent photoelectric performance, and chemical stability, abrasion resistance, to advantages such as biological nontoxics, nano titanium oxide has been widely used in the preparation of gas sensor, pressure-active element, solar cell, nonlinear optical material and surrounding purifying material etc.The titanium dioxide that occurring in nature exists mainly contains three kinds of crystal formations: brookite, anatase octahedrite and rutile, synthetic be mainly back two kinds.Recent result of study shows that the photocatalytic activity that contains the titanium dioxide of anatase octahedrite and rutile mixing crystalline phase will be higher than pure anatase octahedrite or pure rutile-phase titanium dioxide (D.S.Muggli, L.Ding, Appl.Catal.B:Environmental, 2001; 32:181), and mix the photocatalytic activity of titanium dioxide of crystalline phase and ratio closely related (R.R.Bacsa, J.Kiwi, Appl.Catal.B:Environmental, 1998 of two crystalline phases; 16:19).Usually the method for employing high-temperature roasting prepares titanium dioxide (Gao Wei, Wu Fengqing, Luo Zhen, Fu Juxia, Wang Dejun, Xu Baokun, SCI, 2001 of anatase octahedrite and rutile mixing crystalline phase; 22:660), but the crystalline phase ratio is difficult to control, and high-temperature roasting energy consumption height, and the titanium dioxide that obtains is easily reunited, and grain-size exceeds nanometer range.How to prepare the nano-titania particle that mixes crystalline phase and become the interested problem of people.Document once reported utilize dissimilar titanium ester as presoma prepared anatase octahedrite mutually with rutile mutually ratio be respectively 0: 100,50: 50,70: 30 nano titanium oxide (R.R.Bacsa, J.Kiwi, Appl.Catal.B:Environmental, 1998; 16:19), but this method preparation cost height, cycle are long, and anatase octahedrite and rutile ratio modulation continuously mutually, are difficult to industry and promote.
Summary of the invention
The purpose of this invention is to provide a kind of anatase octahedrite mutually with the rutile preparation method of the controlled and continuously adjustable nano titanium oxide of ratio mutually.
The preparation method of the controlled titanium dioxide of crystalline phase that the present invention relates to is as follows:
1. titanium-containing compound hydrolysis in alcohol solution prepares amorphous titania.
2. amorphous titania is mixed with certain density mineral acid.
3. the formed colloidal sol of step 2 carries out hydrothermal treatment consists at a certain temperature.
4. hydrothermal treatment consists is after suction filtration, washing, drying obtain the mixed crystal nano titanium oxide.
Said titanium-containing compound general formula is Ti (OR) in 1
nX
4-n(n=0～4), wherein R is C
1-C
4Alkyl, X is a halogens, the halogenide of titanium ester or titanium, for example butyl (tetra) titanate, titanium ethanolate, isopropyl titanate, titanium tetrachloride etc., the water that is added during hydrolysis can respectively be 1～500 and 0～250 with the amount of alcohol and the mol ratio of titanium, when pure titanium ratio is zero, be titanium-containing compound hydrolysis in water.
Said mineral acid such as nitric acid, hydrochloric acid, oxalic acid etc. in 2.Its concentration can be 0～10 mol; The amount that is added can be the amorphous TiO of 5～50ml/g
2
Said treatment process is for to carry out hydrothermal treatment consists in 3 under water vapour self pressure, and the temperature of processing can be 100～240 ℃; The time of handling can be 2～96 hours.
Concentration by the control mineral acid continuously in the modulation nano titanium oxide anatase octahedrite and rutile mix the ratio of crystalline phase, along with the rising of inorganic acid concentration, the raising of rutile mixed crystal phase ratio.Example and figure all obviously show.Different mineral acids is basic identical to the regulation and control of crystalline phase ratio.
Hydrolysis material of the present invention is with butyl (tetra) titanate, titanium ethanolate, and isopropyl titanate or titanium tetrachloride are better, and such raw material sources are many, easily obtain.
The water titanium mol ratio of alcohol solution and pure titanium mol ratio are respectively 10～100 and 5～50 for better during hydrolysis, the reaction efficiency height.
Mineral acid is with hydrochloric acid, and nitric acid or oxalic acid are better, and concentration is in 0～2 mol, and add-on is the amorphous TiO of 10～20ml/g
2The crystalline phase regulating effect is good under this condition, and has reduced reaction cost.
The hydrothermal treatment consists Controllable Temperature is built in 150～200 ℃, the time be 8～48 hours be better treatment condition.
The preparation method's of the titanium dioxide nanocrystalline that crystalline phase provided by the invention is controlled outstanding advantage is:
1, preparation condition gentleness does not need high-temperature roasting can obtain the nano titanium oxide of mixed crystal.
2, preparation equipment and technology are simple, and is with short production cycle, and processing parameter is controlled easily, is easy to industry and promotes.
3, in the nano titanium oxide anatase octahedrite mutually with rutile mutually ratio can carry out continuous modulation by the concentration of control mineral acid.
Description of drawings
Fig. 1 is the XRD figure of the nano titanium oxide of (sample 1-9) preparation under the different condition.
Fig. 2 is an anatase octahedrite phase and rutile ratio mutually in the nano titanium oxide for preparing under the different condition.
Embodiment example 1～9
0.1mol butyl (tetra) titanate is dissolved in the 1.5mol dehydrated alcohol, drips the mixed solution of 1mol ethanol and 5mol water, at room temperature stirs 3 hours, gets the amorphous titania powder through suction filtration, drying at room temperature then.In the amorphous titania powder, add a certain amount of nitric acid (10mL/g titanium dioxide powder), concentration of nitric acid is respectively 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,1.0mol/L, stirred 1 hour under the room temperature, 180 ℃ of hydrothermal crystallizings 24 hours, obtain titanium dioxide sample through suction filtration, washing, drying, be designated as sample 1-9 respectively.Example 10
The XRD figure of working sample 1-9 sample spectrum on Rigaku D/MAX-IIA diffractometer, wherein 25.2,38.7 and 48.0 ° peak belongs to the diffraction of anatase octahedrite (101), (004) and (200) crystal face respectively, and 27.4,36.1,41.2 and 54.3 ° peak belongs to the diffraction of rutile (110), (101), (111) and (211) crystal face respectively.Anatase octahedrite mutually and the rutile quantitative mutually formula x of ratio utilization mutually in the titanium dioxide
A=(1+1.26I
R/ I
A)
-1Calculate (C.C.Wang, J.Y.Ying, Chem.Mater, 1999; 11:3113), x wherein
ABe the mutually shared ratio of anatase octahedrite, I
AAnd I
RBe respectively the intensity that belongs to the diffraction peak of anatase octahedrite and rutile, the results are shown in Table 1.Example 11～12
0.1mol butyl (tetra) titanate is dissolved in the 1.5mol dehydrated alcohol, drips the mixed solution of 1mol ethanol and 5mol water, at room temperature stirs 3 hours, gets the amorphous titania powder through suction filtration, drying at room temperature then.In the amorphous titania powder, add a certain amount of hydrochloric acid (20mL/g titanium dioxide powder), concentration is respectively 0.2,0.3mol/L, stirred 1 hour under the room temperature, 180 ℃ of hydrothermal crystallizings 24 hours, obtain titanium dioxide sample through suction filtration, washing, drying, be designated as sample 11,12 respectively, utilize the method for example 10 to measure the mutually shared ratio of its anatase octahedrite.Example 13～14
The 40ml titanium tetrachloride is dissolved in the 100mL 0.6N hydrochloric acid, and ammoniacal liquor to the pH value that dripped then 1: 1 is 9～10.Ageing is 12 hours under the room temperature, and suction filtration is washed with distilled water to no chlorion after drying, grinding, makes the amorphous titania powder.In the amorphous titania powder, add a certain amount of hydrochloric acid (10mL/g titanium dioxide powder), concentration is 0.3mol/L, stirred 1 hour under the room temperature, 150 ℃ of hydro-thermals are crystallization 24 and 48 hours respectively, obtain titanium dioxide sample through suction filtration, washing, drying, be designated as sample 13,14 respectively, utilize the method for example 10 to measure the mutually shared ratio of its anatase octahedrite.Example 15～18
Method synthesis of nano TiO according to example 1
2Crystal, concrete synthesis condition is as follows, and utilizes the method for example 10 to measure the mutually shared ratio of its anatase octahedrite.
| Raw material | Water/titanium | Alcohol/titanium | Concentration of hydrochloric acid | The acid add-on | The hydrothermal treatment consists temperature | The hydrothermal treatment consists time | Anatase octahedrite phase ratio |
| Titanium ethanolate | ????100 | ????50 | ????2 | ????5 | ??160 | ??48 | ??40 |
| Titanium ethanolate | ????100 | ????50 | ????2 | ????50 | ??180 | ??48 | ??0 |
| Isopropyl titanate | ????100 | ????5 | ????1 | ????5 | ??200 | ??4 | ??75 |
| The metatitanic acid methyl esters | ????10 | ????5 | ????0 | ????5 | ??150 | ??4 | ??100 |
Claims (5)
1, the method for the controlled titanium dioxide nanocrystalline of a kind of crystalline phase, preparation process comprises hydrolysis, the adding of mineral acid, hydrothermal treatment consists, suction filtration, washing, the drying and other steps of titanium-containing compound, it is characterized in that:
(1) the used raw material of hydrolysis is a titanium-containing compound, and its general formula is:
Ti(OR)
nX
4-n(n＝0～4)
R is C in the formula
1-C
4Alkyl, X is a halogens
(2) hydrating solution is an alcohol solution, and water titanium mol ratio and pure titanium mol ratio are respectively 1～500 and 0～250
What (3) added is mineral acid, and its concentration is 0～10 mol, and add-on is the amorphous TiO of 5～50ml/g
2
(4) temperature of hydrothermal treatment consists is 100～240 ℃, and the time is 2～96 hours
2, the method for the controlled titanium dioxide nanocrystalline of crystalline phase according to claim 1 is characterized in that hydrolysis material is any in following: butyl (tetra) titanate, titanium ethanolate, isopropyl titanate, titanium tetrachloride.
3, the method for the controlled titanium dioxide nanocrystalline of crystalline phase according to claim 1 is characterized in that hydrating solution is an alcohol solution, and water titanium mol ratio and pure titanium mol ratio are respectively 10～100 and 5～50.
4, the method for the controlled titanium dioxide nanocrystalline of crystalline phase according to claim 1 is characterized in that the mineral acid that is added is hydrochloric acid or nitric acid or oxalic acid, and its concentration is 0～2 mol, and add-on is the amorphous TiO of 10～20ml/g
2
5, the method for the controlled titanium dioxide nanocrystalline of crystalline phase according to claim 1, the temperature that it is characterized in that hydrothermal treatment consists is 150～200 ℃, the time is 8～48 hours.
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