CN102701275B - Method for preparing TiO2 nano laces - Google Patents

Method for preparing TiO2 nano laces Download PDF

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CN102701275B
CN102701275B CN201210180449.1A CN201210180449A CN102701275B CN 102701275 B CN102701275 B CN 102701275B CN 201210180449 A CN201210180449 A CN 201210180449A CN 102701275 B CN102701275 B CN 102701275B
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tio
solution
lace
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CN102701275A (en
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李美成
姜永健
宋丹丹
丁瑞强
姜冰
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North China Electric Power University
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North China Electric Power University
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Abstract

The invention discloses a method for preparing TiO2 nano laces, and belongs to the technical field of nano materials. According to the method, commercial P25 TiO2 nano particles are adopted, and are synthetized into TiO2 nano belts as precursors in a hydro-thermal method, butyl titanate solution is assed in HCl aqueous solution and uniformly mixed, a certain quantity of TiO2 nano belts is added in a mixed solution and uniformly mixed, then the mixed solution is transferred in a reaction kettle for reacting for 6 to 12 hours at the temperature of 160 to 200 DEG C, washed and dried to obtain the TiO2 nano laces; the P25 TiO2 nano particles, the TiO2 nano belts and the TiO2 nano laces are subject to the silver mixing processing in a silver mirror reaction method to obtain Ag/P25 TiO2 nano particles, Ag/TiO2 nano belts and Ag/TiO2 nano laces, and experiment that methyl orange is subject to photocatalytic degradation shows that Ag/TiO2 nano lace have strongest photocatalytic activity.

Description

A kind of TiO for preparing 2the method of nanometer lace
Technical field
The invention belongs to technical field of nano material, particularly a kind of TiO for preparing 2the method of nanometer lace.
Background technology
TiO 2nano material, has larger specific surface area, excellent charge transport properties, in fields such as photochemical catalysis, dye sensitization solar battery and lithium celies, is widely used.TiO 2nanostructure, comprise nano particle, nano wire, nano-pillar, nano belt and nano flower-like structure etc., embody different performances, attracted numerous research.TiO 2the synthetic method of nanostructure adopts hydrothermal synthesis method conventionally, and this method preparation technology is simple, easy control of reaction conditions.Different nanostructures is controlled by different synthesis conditions, as the hydrolysis rate of titanium compound, concentration, and the pH value of solution etc.Wherein, how to change synthesis condition, obtain the structure that contains a large amount of sharp keen edges and turning, to improving TiO 2photochemistry and catalytic performance are of crucial importance.We by adding the TiO with nanostructure in reactant 2nano belt is as the carrier of reaction, utilizes product after butyl (tetra) titanate hydrolysis at TiO 2the ordering growth on nano belt surface, has obtained a kind of new nanostructure.Existing synthetic method can realize single flower structure, and the synthetic nano belt of this method utilization can realize the synthetic banded bouquet that is similar to as support, the spike flower of a branch of bundle is arranged in a nano belt, thereby be more conducive to obtain large specific surface area, there is a large amount of sharpened edges and turning simultaneously, can obtain excellent photochemistry and photocatalysis performance undoubtedly.
Summary of the invention
The object of the invention is to propose a kind of new preparation TiO 2the method of nanometer lace, method provided by the invention adopts TiO 2nano belt is as the carrier (presoma) of reaction, and adopts simple silver mirror reaction to prepare to mix silver-colored TiO 2nano flower band structure.Concrete preparation method comprises the steps:
(1) prepare TiO 2nano belt:
A. by P25 TiO 2nano particle joins in the NaOH aqueous solution, and magnetic agitation is even, and gained mixing solutions is put into reactor, react 12 ~ 24 hours at 180 ~ 200 ℃, by the washing of gained precipitate with deionized water, suction filtration, to filtrate be neutrality, obtain sodium titanate nano belt;
B. prepare HCl solution, the sodium titanate nano belt that step a is made is soaked in described HCl solution;
C. by step b gained solid matter with deionized water washing, suction filtration, to filtrate, be neutral, then after drying, calcining, acquisition TiO 2nano belt;
(2) according to deionized water: the ratio preparation HCl that the volume ratio of the hydrochloric acid that volume fraction is 37% is 1:1 suppresses solution; According to HCl described in every 17mL, suppressing to add in solution massfraction is again the ratio of butyl (tetra) titanate solution 1 ~ 3mL of 98%, butyl (tetra) titanate solution is joined to described HCl and suppress in solution, is stirred to evenly;
(3) TiO that adds appropriate step (1) to make in step (2) gained solution 2nano belt, continues to be stirred to evenly;
(4) step (3) gained solution is transferred in reactor, reacts 6 ~ 12 hours at 160 ~ 200 ℃;
(5) by reacted precipitate with deionized water and absolute ethanol washing to filtrate, be neutral, then carry out drying treatment, obtain TiO 2nanometer lace;
(6) under room temperature, prepare silver ammino solution: in reaction vessel, splash into silver nitrate solution, the concentration of silver nitrate solution is controlled between 1wt% ~ 2wt%; In reaction vessel, drip gradually concentration at the ammoniacal liquor of 1wt% ~ 2wt% again, the PH in reaction vessel is controlled between 8 ~ 9, and constantly concussion, until the precipitation producing disappears just;
(7) by the TiO making 2nanometer lace adds in silver ammino solution prepared by step (6), then dropwise adds the glucose solution of 0.1 ~ 0.3mol/L, reacts 8 ~ 10min; By deionized water wash, the suction filtration for compounding substances that obtain, until filtrate is neutral, and then through vacuumize dry after, obtain Ag/TiO 2nanometer lace.
The TiO that described step (1) makes 2nano belt, length can reach tens microns, and width is 50 ~ 200 nanometers, and thickness is in 50 nanometer left and right;
The concentration of the NaOH solution using in described step (1) is 10mol/L, and the concentration of HCl solution is 0.1 mol/L, to guarantee carrying out completely of reaction;
Drying temperature in described step (1) is 50 ~ 70 ℃, and be 1 ~ 3 hour time of drying; Calcining temperature is 550 ~ 650 ℃, and calcination time is 1 ~ 3 hour;
The TiO adding in described step (3) 2the weight of nano belt is: in every use step (2), 17mL HCl suppresses solution, the TiO that adds 0.01 ~ 0.05g step (1) to make 2nano belt;
Drying treatment in described step (5) is: drying temperature is 80 ℃, and be 12 hours time of drying.
Beneficial effect of the present invention is:
The present invention adopts industrial TiO 2particle (P25), first utilizes hydrothermal method synthesis of titanium dioxide nano belt, the advantage of Hydrothermal Synthesis be can in warm liquid phase control, energy consumption is relatively low, controllability good and carry out in airtight container, pollutes little; The TiO that utilizes method provided by the present invention to prepare 2nanometer lace has a lot of sharpened edges and turning, can effectively improve TiO 2photochemistry and photocatalysis performance; To TiO 2the test of nanometer lace shows, TiO 2nano flower band structure has very large specific surface area; According to the photodegradation experiment of carrying out, show TiO 2nanometer lace is better than TiO to the photocatalysis effect of tropeolin-D 2with P25 and TiO 2nano belt; Due to TiO 2nanometer lace has large specific surface area and stronger photocatalytic activity, therefore can be widely used in the fields such as photochemistry, lithium cell test, dye sensitization and solar cell.
Accompanying drawing explanation
Fig. 1 is new Ti O synthetic in the embodiment of the present invention 2the scanning electron microscope diagram of nano flower band structure;
Fig. 2 is Ag/P25, Ag/TiO synthetic in the embodiment of the present invention 2nano belt and Ag/TiO 2the comparative test result of the Photocatalytic Degradation On Methyl Orange Solution of nanometer lace.
Embodiment
A kind of method of preparing nano titania lace that the present invention proposes can be implemented by following method, and concrete preparation method comprises the steps:
(1) prepare TiO 2nano belt:
A. by P25 TiO 2nano particle joins in the NaOH aqueous solution that concentration is 10mol/L, and magnetic agitation is even, and gained mixing solutions is put into reactor, react 12 ~ 24 hours at 180 ~ 200 ℃, by the washing of gained precipitate with deionized water, suction filtration, to filtrate be neutrality;
B. the HCl solution that compound concentration is 0.1mol/L, is soaked in step a gained throw out in described HCl solution;
C. by the washing of step b gained solid matter with deionized water, suction filtration, to filtrate, be neutral; Then in temperature, it is under the condition of 50 ~ 70 ℃ dry 1 ~ 3 hour; Finally under temperature is the condition of 550 ~ 650 ℃, calcine after 1 ~ 3 hour, obtain TiO 2nano belt;
(2) according to deionized water: the ratio preparation HCl that the volume ratio of the hydrochloric acid that volume fraction is 37% is 1:1 suppresses solution; According to HCl described in every 17mL, suppressing to add in solution massfraction is again the ratio of butyl (tetra) titanate solution 1 ~ 3mL of 98%, butyl (tetra) titanate solution is joined to described HCl and suppress in solution, is stirred to evenly;
(3) according to 17mL HCl in every use step (2), suppress solution, the TiO that adds 0.01 ~ 0.05g step (1) to make 2the ratio of nano belt, the TiO that step (1) is made 2nano belt joins the HCl inhibition solution that step (2) makes, and continues to be stirred to evenly;
(4) step (3) gained solution is transferred in reactor, reacts 6 ~ 12 hours at 160 ~ 200 ℃;
(5) reacted precipitate with deionized water and alcohol are washed to filtrate as neutral, then at 80 ℃ dry 12 hours, obtain TiO 2nanometer lace;
(6) under room temperature, prepare silver ammino solution: in reaction vessel, splash into silver nitrate solution, the concentration of silver nitrate solution is controlled between 1wt% ~ 2wt%; In reaction vessel, drip gradually concentration at the ammoniacal liquor of 1wt% ~ 2wt% again, the PH in reaction vessel is controlled between 8 ~ 9, and constantly concussion, until the precipitation producing disappears just;
(7) by the TiO making 2nanometer lace adds in silver ammino solution prepared by step (6), then dropwise adds the glucose solution of 0.1 ~ 0.3mol/L, reacts 8 ~ 10min; By deionized water wash, the suction filtration for compounding substances that obtain, until filtrate is neutral, and then through vacuumize dry after, obtain Ag/TiO 2nanometer lace.
Below in conjunction with specific embodiment, the present invention is described in detail:
Embodiment 1:
(1) prepare TiO 2nano belt:
A. by 1g P25 TiO 2nano particle joins in the NaOH aqueous solution that 100mL concentration is 10mol/L, and magnetic agitation is even, and gained mixing solutions is put into reactor, react 24 hours at 200 ℃, by the washing of gained precipitate with deionized water, suction filtration, to filtrate be neutrality;
B. the HCl solution 250mL that compound concentration is 0.1mol/L, is soaked in step a gained throw out in described HCl solution;
C. by the washing of step b gained solid matter with deionized water, suction filtration, to filtrate, be neutral; Then under the condition of 60 ℃, be dried 2 hours, finally under the condition of 600 ℃, calcine after 2 hours, obtain TiO 2nano belt;
(2), according to deionized water: ratio that the volume ratio of the hydrochloric acid that volume fraction is 37% is 1:1 preparation HCl suppresses solution 17mL, then to described HCl, suppressing to add in solution massfraction is 98% butyl (tetra) titanate solution 1.5mL, is stirred to evenly;
(3) TiO that adds 0.02g step (1) to prepare in above-mentioned solution 2nano belt, continues to stir 10min left and right to even;
(4) step (3) gained solution is transferred in reactor, reacts 6 hours at 160 ℃;
(5) reacted precipitate with deionized water and alcohol are washed to filtrate as neutral, then at 80 ℃ dry 12 hours, obtain TiO as shown in Figure 1 2nanometer lace;
(6) under room temperature, prepare three parts of the silver ammino solutions of 0.2mol/L, weigh respectively the P25 TiO of 0.1g 2nano particle, TiO prepared by step (1) 2nano belt and TiO 2nanometer lace is placed in respectively silver ammino solution;
(7) glucose solution of 0.3mol/L is dropwise splashed in solution prepared by step (6) to silver mirror reaction 10min; Three parts of compounding substances that obtain are used respectively to deionized water wash, suction filtration, until filtrate is neutral, then under 80 ℃ of conditions, is dried and after 6 hours, obtains Ag/P25, Ag/ TiO 2nano belt and Ag/ TiO 2nanometer lace;
(8) by the Ag/P25 making in step (7), Ag/ TiO 2nano belt and Ag/ TiO 2nanometer lace carries out respectively the experiment of photo-catalytic degradation of methyl-orange, and concrete grammar is as follows: the methyl orange solution that under room temperature, configuration concentration is 0.02g/L; Get three parts of methyl orange solutions prepared by 20mL, the Ag/P25 respectively 0.02g being made, Ag/ TiO 2nano belt and Ag/TiO 2nanometer lace joins in described methyl orange solution, and then UV illumination 60min carries out photoabsorption test to the sample obtaining.As shown in Figure 2, result shows result: Ag/ TiO 2nanometer lace presents the strongest photocatalytic activity, simultaneously Ag/ TiO 2the photocatalysis performance of nano belt is also better than Ag/ P25.
Embodiment 2,3,4,5:
The TiO that the step (1) adding in embodiment 1 step (3) is made 2nano belt changes 0.01g, 0.03g, 0.04g or 0.05g into, and other conditions, with embodiment 1, can obtain technique effect as repeated faithfully in Example 1.

Claims (4)

1. prepare TiO for one kind 2the method of nanometer lace, is characterized in that, concrete preparation method comprises the steps:
(1) prepare TiO 2nano belt:
A. by 1g P25TiO 2nano particle joins in the NaOH aqueous solution that 100mL concentration is 10mol/L, and magnetic agitation is even, and gained mixing solutions is put into reactor, at 180～200 ℃, react 12～24 hours, by the washing of gained precipitate with deionized water, suction filtration, to filtrate, be neutral, obtain sodium titanate nano belt;
B. the HCl solution 250mL that compound concentration is 0.1mol/L, the sodium titanate nano belt that step a is made is soaked in described HCl solution;
C. by step b gained solid matter with deionized water washing, suction filtration, to filtrate, be neutral, then after drying, calcining, acquisition TiO 2nano belt;
(2) according to deionized water: the ratio preparation HCl that the volume ratio of the hydrochloric acid that volume fraction is 37% is 1:1 suppresses solution; According to HCl described in every 17mL, suppressing to add in solution massfraction is again the ratio of butyl (tetra) titanate solution 1～3mL of 98%, butyl (tetra) titanate solution is joined to described HCl and suppress in solution, is stirred to evenly;
(3) TiO that adds appropriate step (1) to make in step (2) gained solution 2nano belt, continues to be stirred to evenly; The TiO adding 2the ratio of nano belt is: in every use step (2), 17mL HCl suppresses solution, the TiO that adds 0.01～0.05g step (1) to make 2nano belt;
(4) step (3) gained solution is transferred in reactor, reacts 6～12 hours at 160～200 ℃;
(5) by reacted precipitate with deionized water and absolute ethanol washing to filtrate, be neutral, then carry out drying treatment, obtain TiO 2nanometer lace.
2. preparation TiO according to claim 1 2the method of nanometer lace, is characterized in that, described in step (1), dry drying temperature is 50～70 ℃, and be 1～3 hour time of drying; The calcining temperature of described calcining is 550～650 ℃, and calcination time is 1～3 hour.
3. preparation TiO according to claim 1 2the method of nanometer lace, is characterized in that, the drying treatment in described step (5) is: drying temperature is 80 ℃, and be 12 hours time of drying.
4. preparation TiO according to claim 1 2the method of nanometer lace, is characterized in that, described TiO 2nanometer lace is through silver-plated processing, and described silver-plated processing comprises the steps:
(1) in reaction vessel, splash into silver nitrate solution, the concentration of silver nitrate solution is controlled between 1wt%～2wt%;
(2) in reaction vessel, drip gradually concentration at the ammoniacal liquor of 1wt%～2wt% again, the pH in reaction vessel is controlled between 8～9, and constantly concussion, until the precipitation producing disappears just;
(3) by the TiO making 2nanometer lace adds in silver ammino solution prepared by step (2), then dropwise adds the glucose solution of 0.1～0.3mol/L, reacts 8～10min; By deionized water wash, the suction filtration for compounding substances that obtain, until filtrate is neutral, and then through vacuumize dry after, obtain Ag/TiO 2nanometer lace.
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CN103318955B (en) * 2013-06-24 2015-08-12 华北电力大学 A kind of string-like TiO 2sphere material and preparation method thereof
CN103691433B (en) * 2013-12-10 2016-01-20 北京科技大学 A kind of Ag doped Ti O 2material, and its preparation method and application
CN103752312B (en) * 2013-12-26 2016-01-20 深圳大学 A kind of photochemical catalyst and preparation method thereof
CN103880072B (en) * 2014-03-24 2016-01-06 华北电力大学 A kind of preparation method of pinecone shape titanium dioxide nano material
CN104190458B (en) * 2014-07-16 2016-08-24 上海工程技术大学 A kind of low temperature preparation technology of dual element modified nano-titanium dioxide colloidal sol
CN105177671B (en) * 2015-08-19 2018-05-08 苏州榕绿纳米科技有限公司 A kind of preparation method of silver Nano granule/titanium dioxide nano-tube array
CN106582591A (en) * 2016-11-17 2017-04-26 广东工业大学 Preparation method of quadrangular anatase type TiO2
CN107389736A (en) * 2017-05-22 2017-11-24 江苏时瑞电子科技有限公司 A kind of preparation method of the humidity sensor based on sodium titanate
CN107308927A (en) * 2017-06-28 2017-11-03 陕西科技大学 A kind of preparation method of titanium dioxide homojunction nano-photocatalyst

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