CN105271400A - Preparation method of mixed crystal nano-TiO2 - Google Patents
Preparation method of mixed crystal nano-TiO2 Download PDFInfo
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- CN105271400A CN105271400A CN201510890698.3A CN201510890698A CN105271400A CN 105271400 A CN105271400 A CN 105271400A CN 201510890698 A CN201510890698 A CN 201510890698A CN 105271400 A CN105271400 A CN 105271400A
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Abstract
The invention relates to a preparation method of mixed crystal nano-TiO2. The method includes the steps that TiCl4 of a certain volume is slowly dissolved in deionized water; the TiCl4 solution is continuously aged for certain time at a low temperature section (30-60 DEG C) and a high temperature section (60-90 DEG C) after being stabilized, wherein no additive is needed, and the rutile phase content (16.8-75.6%) in a final product is regulated and controlled just by controlling the aging time of the TiCl4 solution at the low temperature and the high temperature; finally, obtained precipitates are filtered, washed and dried to obtain the mixed crystal nano-TiO2 powder with different rutile-anatase proportions.
Description
Technical field
The present invention relates to field of nanometer material technology, more specifically, relate to a kind of preparation method of mixed phase nano-titania.
Background technology
In recent years, environment and energy problem caused showing great attention to of people.In huge textile industry production process, dyestuff becomes organic pollutant very serious in ecotope, and be difficult to removing by method that is biological and physics, photocatalytic pollutant degradation is considered to effective means always.And nano titanium oxide is as a kind of nontoxic, cheap and nano material of stable in properties, be expected to become the most promising photocatalyst.
Nano titanium dioxide, also known as titanium dioxide, diameter is below 100 nanometers, and product appearance is fluffy white powder.TiO
2nano particle stable in properties, it is good to catch optical property, recoverable.TiO
2application Areas also boundless, be widely used in the aspects such as energy and environment, biological aspect, medical treatment and health, there is following advantage:
1, photocatalytic pollutant degradation: nano-TiO
2as catalyzer, there is no secondary pollution and there is no selectivity, being widely used in environmental pollution aspect.Can degradation of dye waste water, sterilant, agricultural chemicals waste water, tensio-active agent, also has the trade effluent containing heavy metal, can oxidizedly degrade;
2, the application of dye sensitization solar battery aspect: semiconductor nano TiO
2there is broader energy gap, and good light fastness.Dyestuff photosensitive molecular is adsorbed on semiconductor nano TiO
2surface, improve photoelectric transformation efficiency;
3, nano-TiO
2to ultraviolet shielding effect: nano-TiO
2there is certain shielding effect to ultraviolet, add the features such as it is nontoxic, stable in properties, make nano-TiO
2be applied to sun-proof, all respects such as coating, man-made fiber, rubber, plastics of makeup.
Nano titanium oxide mainly contains two kinds of crystal habits: anatase titanium dioxide (Anatase) and rutile-type (Rutile).Rutile titanium dioxide is more stable and fine and close than anatase titanium dioxide, and have higher hardness, density, specific inductivity and specific refractory power, its opacifying power and tinting strength are also higher.And anatase titanium dioxide is high at the luminance factor rutile titanium dioxide of visible ray shortwave part, band blue color, and lower than rutile-type to ultraviolet receptivity, photocatalytic activity is higher than rutile-type.Under certain condition, anatase titanium dioxide can be converted into rutile titanium dioxide.
In the existing preparation process of mixed phase nano-titania, in order to prepare qualified nanometer titanium dioxide titanium products, often in preparation process, add precipitation agent and heat-treat, as: (the Wang Wei such as Wang Wei, Ruan Chengdong, Ru Hongqiang, a kind of mesoporous TiO 2 color material and preparation method thereof, China, patent of invention, 201410231843.2, 2014.08.13) with titanium source (titanium tetrachloride, titanous chloride, one or both in titanic acid ester) to react with water and prepare metatitanic acid, metatitanic acid and hydrogen peroxide are mixed with out titanium peroxide acid, nonionic surface active agent and peroxidation metatitanic acid are formed matrix material, and matrix material is carried out roasting obtain mesoporous TiO 2.(the Wang Bing such as Wang Bing, Yang Zewei, An Hao, Deng. the low temperature preparation method of a kind of brookite and rutile titanium dioxide nanometer mixed crystal. China, patent of invention, 201410629923.3,2015.03.25) ultrapure water, tetraethyl titanate and dehydrated alcohol be mixed with by a certain percentage and obtain hydrous titanium oxide after drying, add hydrogen peroxide and obtain peroxo titanic acid sol, by colloidal sol water-bath at 40 ~ 60 DEG C, finally under the condition of 160 ~ 200 DEG C, carry out hydro-thermal reaction, namely product obtains mixed crystal after washing drying.Wang Zhenxing etc. (Wang Zhenxing, Ding Shiwen, Zhang Meihong. a synthesis of high-dispersion nano titanium dioxide mixed crystal! Structure and photocatalysis performance, Chinese Journal of Inorganic Chemistry, 2005,3,21) in stink cupboard, measure titanium tetrachloride with dry graduated cylinder slowly join in hydrochloric acid soln.Again the aqueous solution being dissolved with a certain amount of urea is added in solution fast after mixing solutions being heated rapidly to 100 DEG C of isothermal reaction 10 ~ 60min.In the basic conditions in 100 DEG C of back flow reaction 2h decompress filters, washing.Then dry, finally put into retort furnace calcination 30min and take out sample.In order to prevent nanoparticle from drying course, hard aggregation occurring, in mixing solutions, add a certain amount of nano level carbon black.Ding Shiwen etc. (Ding Shiwen, Dong Wei, Wang Liyong, etc. mixed crystal nano-TiO
2preparation and Study on degradation to cyanide wastewater, University Of Xiangtan's natural science journal, 2008,2,30.) 11mLTiCl is slowly added drop-wise in 200mL distilled water, keep dripping a fast 1d/s, in titration process, keep solution to clarify.Settled solution in beaker is gone in 500mL three-necked bottle, be heated to boiling in acid condition, occur after muddiness, continuing reaction 10 ~ 60min until solution, then add the ammoniacal liquor adjust ph of 1ml to weakly alkaline, continue reaction 60min.Decompress filter, washing, put roasting 60min in people's muffle furnace after 80 ~ 90 DEG C of dryings obtain powdered sample.Wang Li bravely waits (Wang Liyong, Bai Zhenyu, Dong Wei etc. synthesis and the photodegradation Xylene Red 3R of mixed phase nano-titania study, University Of Hebei's journal (natural science edition), and 2007,3,27) by TiCl
4with in 1 speed instillation 200mL deionized water per second, be rapidly heated, occur a large amount of white casse to system, 100 DEG C reaction for some time after, volume fraction be the ammonia neutralization of 50% to weakly alkaline, 100 DEG C continue reaction 3h after, after filtration, deionized water washes away NH to product
4+and Cl
-foreign ion, then wash away moisture residual in sample with dehydrated alcohol, vacuum-drying, porphyrize, obtained nanometer mixed crystal powder.Season gold careless to wait (season gold careless, Guo Jing, Shi Chaohui, etc. the preparation of mixed crystal form nanometer titanium dioxide turbid liquor and photocatalysis performance thereof. material Leader B: a research section, 2012,7,26) in the mixing solutions of ammoniacal liquor and water, drip TiCl
4solution, high temperature oil bath is heated, and uses concentrated hydrochloric acid adjust ph, can obtain white precipitate TiO
2.(the Du Jinge such as Du Jinge, Yao Chaozong. the preparation of nano titanium oxide and photocatalysis performance thereof, chemical research, 2012,4,23) titanium tetrachloride is joined in the mixing solutions of distilled water and ethanol, stir, slowly drip urea soln, after room temperature at the uniform velocity stirs 2h, be transferred in teflon-lined autoclave, 180 DEG C of constant temperature process 16h in air dry oven.Be cooled to room temperature, filter, wash, 60 DEG C of oven dry, namely obtain TiO
2nano-powder.In the preparation process of mixed phase nano-titania, bronsted lowry acids and bases bronsted lowry is participated in preparation process by as precipitation agent, and follow-up heat treatment process too increases the complicacy of preparation process.The present invention, by preparing the controlled mixed crystal nano silicon of crystal form ratio when not adding precipitation agent and carrying out subsequent heat treatment to temperature of reaction and the control in reaction times, reduces the complicacy of preparation process.
Summary of the invention
In view of the above problems, the invention provides a kind of preparation method of mixed phase nano-titania, in a preparation process, the titanium dioxide of anatase titanium dioxide and rutile-type mixing crystal formation can be obtained simultaneously.Concrete technical scheme is as follows:
A preparation method for mixed phase nano-titania, is characterized in that, comprises the following steps:
First, by TiCl
4be dissolved in deionized water, be mixed with certain density TiCl
4the aqueous solution; Then, under the low temperature of 30 ~ 60 DEG C aging 2 ~ 8h and/or under the high temperature of 60 ~ 90 DEG C aging 2 ~ 8h, the throw out that obtains to be filtered, washing, dry, in the process, not to need to add any reagent and adjust ph; Finally, described mixed phase nano-titania is obtained;
Described TiCl
4be 1:100 ~ 1:30 with the volume ratio of deionized water.
Described mixed crystal refers to the mixing of anatase titanium dioxide and rutile-type two kinds of crystal formations.
Weight ratio 10 ~ 80:20 ~ 90 of described anatase titanium dioxide and rutile-type.
Present inventor finds after deliberation, and the reason that mixed crystal generates may be that two kinds of crystal formations formation speed is at different temperatures different: during low temperature, and it is very fast that rutile-type grows; During high temperature, it is very fast that anatase titanium dioxide grows.So rutile content is high in the mixed crystal generated when low temperature, after high―temperature nuclei, anatase content is high.In order to regulate the ratio of mixed crystal, adopting at low high temperature two temperature sections, different growth times, reaching the object regulating mixed crystal ratio.
Advantage of the present invention and beneficial effect as follows: nano-titanium oxide is a kind of excellent photocatalyst material, particularly there is a certain proportion of mixed crystal titanium oxide, traditional method is the ratio by changing calcining temperature and calcination time or the method regulation and control mixed crystal by some chemical additives of interpolation, calcining easily causes sintering and the reunion of particle, and the method operating process adding control agent is complicated; And preparation method provided by the invention, only need TiCl
4be dissolved in water, be made into a certain proportion of aqueous solution, at different temperature the aging different time, just can regulate and control the ratio of sharp titanium and rutile in product.The method preparation process is simple, and the slurry obtained can directly be carried on carrier, avoids the reunion in calcination process.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the mixed crystal titanium dioxide of embodiment 1;
Fig. 2 is the X-ray diffraction matching collection of illustrative plates of the mixed crystal titanium dioxide of embodiment 1;
Fig. 3 is the X ray diffracting spectrum of the mixed crystal titanium dioxide of embodiment 2;
Fig. 4 is the X-ray diffraction matching collection of illustrative plates of the mixed crystal titanium dioxide of embodiment 2;
Fig. 5 is the X ray diffracting spectrum of the mixed crystal titanium dioxide of embodiment 3;
Fig. 6 is the X-ray diffraction matching collection of illustrative plates of the mixed crystal titanium dioxide of embodiment 3;
Fig. 7 is the X ray diffracting spectrum of the mixed crystal titanium dioxide of embodiment 4;
Fig. 8 is the X-ray diffraction matching collection of illustrative plates of the mixed crystal titanium dioxide of embodiment 4;
Fig. 9 is the X ray diffracting spectrum of the mixed crystal titanium dioxide of embodiment 5;
Figure 10 is the X-ray diffraction matching collection of illustrative plates of the mixed crystal titanium dioxide of embodiment 5;
Figure 11 is the X ray diffracting spectrum of the mixed crystal titanium dioxide of embodiment 6;
Figure 12 is the X-ray diffraction matching collection of illustrative plates of the mixed crystal titanium dioxide of embodiment 6.
Embodiment
Below by embodiment, the present invention is specifically described.What be necessary to herein means out is that following examples are only for the invention will be further described; limiting the scope of the invention can not be interpreted as; some nonessential improvement and adjustment that professional and technical personnel's content according to the present invention in this field is made, still belong to protection scope of the present invention.
Embodiment 1
By the TiCl of 3.5mL
4be dissolved in 100mL deionized water.6h is heated in the water bath with thermostatic control of solution being put into 45 DEG C.Subsequently gained slurry carried out filtering, wash, dry, obtain mixed crystal titanium oxide powder.The diffracting spectrum that products obtained therefrom records and matching collection of illustrative plates are respectively as depicted in figs. 1 and 2.Calculation of correlation data are as follows:
The content calculating sharp titanium phase in titanium dioxide sample is 24.4%, and median size is 1.10nm.The content of Rutile Type is 75.6%, and median size is less than 1nm.
Embodiment 2
By the TiCl of 2.5mL
4be dissolved in 100mL deionized water.2h is heated in the water bath with thermostatic control of solution being put into 35 DEG C, and 6h is heated in the water bath with thermostatic control of again solution being put into 85 DEG C after taking-up.Subsequently gained slurry carried out filtering, wash, dry, obtain mixed crystal titanium oxide powder.The diffracting spectrum that products obtained therefrom records and matching collection of illustrative plates are respectively as shown in Figure 3 and Figure 4.Calculation of correlation data are as follows:
The content calculating sharp titanium phase in titanium dioxide sample is 72.3%, and median size is less than 1nm.The content of Rutile Type is 27.7%, and median size is 1.06nm.
Embodiment 3
By the TiCl of 2mL
4be dissolved in 100mL deionized water.4h is heated in the water bath with thermostatic control of solution being put into 55 DEG C, and 4h is heated in the water bath with thermostatic control of again solution being put into 80 DEG C after taking-up.Subsequently gained slurry carried out filtering, wash, dry, obtain mixed crystal titanium oxide powder.The diffracting spectrum that products obtained therefrom records and matching collection of illustrative plates are respectively as shown in Figure 5 and Figure 6.Calculation of correlation data are as follows:
The content calculating sharp titanium phase in titanium dioxide sample is 66.7%, and median size is less than 1nm.The content of Rutile Type is 33.3%, and median size is 1.34nm.
Embodiment 4
By the TiCl of 3.5mL
4be dissolved in 100mL deionized water.8h is heated in the water bath with thermostatic control of solution being put into 80 DEG C.Subsequently gained slurry carried out filtering, wash, dry, obtain mixed crystal powder.The diffracting spectrum that products obtained therefrom records and matching collection of illustrative plates are respectively as shown in Figure 7 and Figure 8.Calculation of correlation data are as follows:
The content calculating sharp titanium phase in titanium dioxide sample is 83.2%, and median size is less than 1nm.The content of Rutile Type is 16.8%, and median size is 1.51nm.
Embodiment 5
By the TiCl of 3mL
4be dissolved in 100mL deionized water.2h is heated in the water bath with thermostatic control of solution being put into 70 DEG C, and 6h is heated in the water bath with thermostatic control of again solution being put into 45 DEG C after taking-up.Subsequently gained slurry carried out filtering, wash, dry, obtain mixed crystal titanium oxide powder.The diffracting spectrum that products obtained therefrom records and matching collection of illustrative plates are respectively as shown in Figure 9 and Figure 10.Calculation of correlation data are as follows:
The content calculating sharp titanium phase in titanium dioxide sample is 78.7%, and median size is less than 1nm.The content of Rutile Type is 21.3%, and median size is less than 1nm.
Embodiment 6
By the TiCl of 1.5mL
4be dissolved in 100mL deionized water.Solution is put into the aging 4h of water bath with thermostatic control of 80 DEG C, after taking-up, again solution is put into the aging 4h of water bath with thermostatic control of 45 DEG C.Subsequently gained slurry carried out filtering, wash, dry, obtain mixed crystal titanium oxide powder.The diffracting spectrum that products obtained therefrom records and matching collection of illustrative plates are respectively as is illustrated by figs. 11 and 12.Calculation of correlation data are as follows:
The content calculating sharp titanium phase in titanium dioxide sample is 80%, and median size is less than 1nm.The content of Rutile Type is 20%, and median size is 1.42nm.
Claims (4)
1. a preparation method for mixed phase nano-titania, is characterized in that, comprises the following steps:
First, by TiCl
4be dissolved in deionized water, be mixed with certain density TiCl
4the aqueous solution; Then, under the low temperature of 30 ~ 60 DEG C aging 2 ~ 8h and/or under the high temperature of 60 ~ 90 DEG C aging 2 ~ 8h, the throw out that obtains to be filtered, washing, dry, finally, obtains described mixed phase nano-titania;
Described TiCl
4be 1:100 ~ 1:30 with the volume ratio of deionized water.
2. preparation method according to claim 1, is characterized in that, described mixed crystal refers to the mixing of anatase titanium dioxide and rutile-type two kinds of crystal formations.
3. preparation method according to claim 2, is characterized in that, weight ratio 10 ~ 80:20 ~ 90 of described anatase titanium dioxide and rutile-type.
4. the preparation method of mixed phase nano-titania according to claim 1, is characterized in that, TiCl
430 ~ 60 DEG C of stages of low temperature of aqueous solution weathering process and 60 ~ 90 DEG C of stages of high temperature, may be used alone, can also be used in combination, total digestion time is 4 ~ 8h.
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| CN113882019A (en) * | 2021-09-13 | 2022-01-04 | 华东理工大学 | Method for regulating and controlling titanium dioxide crystal form |
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