CN106745218B - A kind of high-temperature stable titania nanotube raw powder's production technology - Google Patents
A kind of high-temperature stable titania nanotube raw powder's production technology Download PDFInfo
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Abstract
The invention discloses a kind of high-temperature stable titania nanotube raw powder's production technology,Titanate radical nanopipe powder is prepared by hydrothermal synthesis method first,Then it is surface-modified,High-temperature roasting obtains earth silicon/titanic oxide composite nano tube powder,Finally etching removes silica in low-concentration sodium hydroxide solution,Obtain high-temperature stable titania nanotube powder,The titania nanotube powder can keep good tubular morphology at a high temperature of higher than 400 DEG C,With preferable anatase crystal and excellent catalytic effect,It can be widely applied to photocatalysis,Lithium battery,Solar cell,Confinement is catalyzed,Medicine,The fields such as catalysis burning,The prior art is solved directly higher than 400 DEG C of roasting titanate radical nanopipes so that the titania nanotube sintering that surface or interlayer are dehydrated and cause,The problem of fracture is even caved in.
Description
Technical field：
The present invention relates to new energy materials and catalysis material technical field, and in particular to a kind of high-temperature stable titanium dioxide is received
Mitron raw powder's production technology.
Background technology：
It is this that there is good chemical to stablize since Kasuga in 1998 et al. prepares titania nanotube first
The one-dimensional tubular nanometer material of a variety of good characteristics such as property, catalytic activity, wet sensitive, air-sensitive, opto-electronic conversion effect causes people
Extensive concern.Titania nanotube has specific physical chemical property at the same time, such as larger specific surface area, excellent ion
Switching performance, special pore volume and aperture structure, have in fields such as photocatalysis, lithium battery, solar cell, functional materials
Wide application prospect.
Titania nanotube powder has a variety of preparation methods, as template, organic solution anodizing and hydro-thermal are closed
Cheng Fa.Wherein hydrothermal synthesis method due to its preparation method it is simple, the advantages that synthesis of titanium dioxide nanotube purity is high, is made extensively
With, while many scholars study the synthesis condition of titania nanotube, formation mechenism and roasting crystallization mechanism.Always
Well known, anatase phase titanium dioxide has higher catalytic activity and relatively low electron-hole recombination rate, (brilliant in other conditions
Particle size, surface characteristic, specific surface area, pattern) it is constant under conditions of improved, it is necessary to carry out high-temperature roasting to titanate radical nanopipe
Its crystal form further improves its activity.But titania nanotube structure is very sensitive for temperature, when calcination temperature is higher than 400
DEG C when, titania nanotube pattern will sinter, be broken or even cave in, and form anatase titania nano particle, limitation
Its application.Therefore the titania nanotube powder with high-temperature stability is prepared with its necessity.
The content of the invention：
The object of the present invention is to provide a kind of high-temperature stable titania nanotube raw powder's production technology, this method is first
Titanate radical nanopipe powder is prepared by hydrothermal synthesis method, then surface-modified, high-temperature roasting obtains earth silicon/titanic oxide
Composite nano tube powder, finally etching removes silica in low-concentration sodium hydroxide solution, obtains high-temperature stable titanium dioxide
Titanium nanotube dust, the titania nanotube powder can keep good tubular morphology at a high temperature of higher than 400 DEG C, tool
There are preferable anatase crystal and excellent catalytic effect, can be widely applied to photocatalysis, lithium battery, solar cell, confinement
Catalysis, medicine, catalysis burning etc. field, solve the prior art directly higher than 400 DEG C roasting titanate radical nanopipes cause surface or
The problem of titania nanotube that interlayer is dehydrated and causes sinters, fracture is even caved in.
The present invention is achieved by the following technical programs：
A kind of high-temperature stable titania nanotube raw powder's production technology, this method comprise the following steps：
1) hydrothermal synthesis method prepares titanate radical nanopipe powder：Titanic oxide nano is added to the hydroxide of 9-15moL/L
In sodium solution, 110~130 DEG C of stirrings are lower to carry out 12~48h of hydro-thermal reaction, naturally cools to room temperature, filtering, deionized water washing
It is 7 to washing lotion PH, the hydrochloric acid solution of 0.1~0.5moL/L is added in above-mentioned powder, stirring or 2~3h of ultrasound, is used again
It is 7 that deionized water, which is washed to washing lotion PH, and filtering, gained powder is finally dried obtain metatitanic acid nanometer under the conditions of 50~60 DEG C
Pipe；
2) surface modification, high-temperature roasting prepare earth silicon/titanic oxide composite nano tube powder, selected from following two sides
Any one in method：
Method one：The titanate radical nanopipe that step 1) is obtained is dispersed in deionized water solution, is stirred and is dripped into solution
Add volume fraction to be 5~8% glacial acetic acid until the pH value of solution is 3~4, be stirred at room temperature after 1~2h add it is silane coupled
Agent ethanol solution, then stirs 3.5~5h, filtering in 75~85 DEG C of constant temperature, and it is 7 that deionized water, which is washed to washing lotion PH, 50~
Dried under the conditions of 60 DEG C, be subsequently placed in Muffle furnace 1~2h of roasting under the conditions of 425~550 DEG C, obtain silica/bis-
Titanium oxide composite nano tube powder；The mass volume ratio of titanate radical nanopipe and silane coupling agent ethanol solution is 0.5~2g:30~
150mL；It is 1 to state the volume ratio of silane coupling agent and ethanol in silane coupling agent ethanol solution:50~150.
Method two：The titanate radical nanopipe ultrasonic agitation that step 1) obtains is dispersed in 80~100mL deionized water solutions
Solution A is formed, 0.75-2 grams of cetyl trimethylammonium bromide is dissolved in 10~15mL deionized water solutions and forms solution
B, 0.6-2.5mL ethyl orthosilicates are dissolved in 80~100mL ethanol solutions and form solution C, and solution B is slowly added dropwise to
1.5~2h is stirred in solution A and under 0.08~0.1MPa；Then solution C is slowly added dropwise to again, under normal pressure lower stirring
1.5~2h, then by the ammonia spirit that 3~5mL volume fractions are 15~25% be slowly added dropwise into, under normal pressure lower stirring 1.5~
2h, filtering, ethanol solution washing, dries under the conditions of 50~60 DEG C, is subsequently placed in Muffle furnace in 425~550 DEG C of conditions
1~2h of lower roasting, obtains earth silicon/titanic oxide composite nano tube powder.
3) etching removes silica and prepares high-temperature stable titania nanotube powder：The titanium dioxide that step 2) is obtained
Silicon/titanium dioxide composite nano tube powder dispersion concentration be 1~1.5moL/L sodium hydroxide solution in, at room temperature stir 3~
4h, filtering, it is 7 that deionized water, which is washed to washing lotion PH, is dried at 50~60 DEG C, that is, obtains high-temperature stable titania nanotube
Powder.
The silane coupling agent is selected from one kind or two in Si-69, KH550, KH560, KH570, KHA-171 or A-172
More than kind.
Preferably, 6-8g anatase titania nano powders are added to the hydrogen of 150~180mL 10moL/L in step 1)
115-120 DEG C of stirring is lower in sodium hydroxide solution carries out 18~36h of hydro-thermal reaction, naturally cools to room temperature, filtering, deionization washing
It is 7 to wash to washing lotion PH, and the hydrochloric acid solution of 0.1~0.5moL/L is added in above-mentioned powder, stirring or 2~3h of ultrasound, again
It is for several times 7 to washing lotion PH to be washed with deionized, and filtering, gained powder is finally dried obtain metatitanic acid under the conditions of 50~60 DEG C
Nanotube.
Beneficial effects of the present invention are as follows：
The present invention prepares titanate radical nanopipe powder by hydrothermal synthesis method first, then utilizes titanate radical nanopipe surface or layer
Between polyhydroxy structure, it is surface-modified, couple a certain amount of silane coupling agent in its hydroxyl surface, high-temperature roasting obtains dioxy
SiClx/titanium dioxide composite nano tube powder, finally etching removes silica in low-concentration sodium hydroxide solution, obtains height
Warm stabilized chlorine titanium nanotube dust, preparation method step is simple, easy to operate, and the titania nanotube powder of preparation exists
Good tubular morphology can be kept under calcination temperature higher than 400 DEG C, and catalytic effect is excellent, can be widely applied to light and urges
The fields such as change, lithium battery, solar cell, confinement catalysis, medicine, catalysis burning, solve the prior art and are directly higher than 400 DEG C
The titania nanotube that roasting titanate radical nanopipe causes surface or interlayer dehydration and causes sinters, fracture is even caved in
Problem.
Brief description of the drawings：
Fig. 1 is the scanning electron microscope (SEM) photograph of high-temperature stable titania nanotube powder prepared in embodiment 1；
Fig. 2 is the transmission electron microscope picture of high-temperature stable titania nanotube powder prepared in embodiment 1；
Fig. 3 is that earth silicon/titanic oxide composite nano tube and high-temperature stable titanium dioxide prepared in embodiment 1 are received
The x-ray photoelectron spectroscopy figure of mitron；
Fig. 4 is that earth silicon/titanic oxide composite nano tube and high-temperature stable titanium dioxide prepared in embodiment 1 are received
The photo-catalytic degradation of methyl-orange efficiency chart of mitron；
Fig. 5 is the scanning electron microscope (SEM) photograph of high-temperature stable titania nanotube prepared in embodiment 2；
Fig. 6 is the transmission electron microscope picture of high-temperature stable titania nanotube prepared in embodiment 2；
Fig. 7 is the XRD diagram of high-temperature stable titania nanotube prepared in embodiment 2；
Fig. 8 is the scanning electron microscope (SEM) photograph of high-temperature stable titania nanotube prepared in embodiment 3；
Fig. 9 is the transmission electron microscope picture of high-temperature stable titania nanotube prepared in embodiment 3.
Embodiment：
It is to further explanation of the invention, rather than limitation of the present invention below.
Embodiment 1：
6g anatase titania nano powders are added in the sodium hydroxide solution that 150mL concentration is 10moL/L, stirring
And be transferred in reaction kettle, hydrothermal temperature is 115 DEG C, and the reaction time is 24~36h, naturally cools to room temperature.Filter, go
Ion water washing is for several times to washing lotion PH ≈ 7.Supernatant is removed, the hydrochloric acid solution of 0.15moL/L is added in above-mentioned powder, is stirred
Mix or ultrasound 2h, the sample after acid treatment is washed with deionized for several times to washing lotion PH ≈ 7, filtering, finally by gained again
Powder is dried under the conditions of 50 DEG C, this product is titanate radical nanopipe powder.
2g titanate radical nanopipes are dispersed in 50mL deionized water solutions, stirs and dropwise addition volume fraction is into solution
5% glacial acetic acid is stirred at room temperature after 1~2h to add 100mL silane coupling agent KH570 ethanol molten until the PH ≈ 3 of solution
Liquid (V silane coupling agents:V ethanol ≈ 1:100) 3.5h then, is stirred under 75 DEG C of constant temperatures, is filtered, deionized water washing number
It is secondary to be dried under the conditions of 50 DEG C, be subsequently placed in Muffle furnace under the conditions of 425 DEG C and roast 1h to washing lotion PH ≈ 7, obtain dioxy
SiClx/titanium dioxide composite nano tube powder, its x-ray photoelectron spectroscopy figure are as shown in Figure 3.It is above-mentioned compound finally to weigh 1.5g
Nanotube is dispersed in the sodium hydroxide solution that 30mL concentration is 1moL/L, and 3h is stirred at room temperature, and is filtered, deionized water washing
For several times to washing lotion PH ≈ 7, dried under the conditions of 50 DEG C, that is, obtain high-temperature stable titania nanotube powder.Its scanning electron microscope
Figure, transmission electron microscope picture, x-ray photoelectron spectroscopy figure difference are as shown in Figure 1, Figure 2, Figure 3 shows.The earth silicon/titanic oxide of preparation
The photo-catalytic degradation of methyl-orange efficiency chart of composite nano tube and high-temperature stable titania nanotube is as shown in figure 4, can by Fig. 1-2
Know, titania nanotube powder manufactured in the present embodiment can keep good tubulose under the calcination temperature higher than 400 DEG C
Pattern, catalytic effect of the present invention is excellent as shown in Figure 4.
Embodiment 2：
7g anatase titania nano powders are added in the sodium hydroxide solution that 175mL concentration is 10moL/L, stirring
And be transferred in reaction kettle, hydrothermal temperature is 115 DEG C, and the reaction time is 20~30h, naturally cools to room temperature.Filter, go
Ion water washing is for several times to washing lotion PH ≈ 7.Supernatant is removed, the hydrochloric acid solution of 0.1moL/L is added in above-mentioned powder, is stirred
Mix or 2~3h of ultrasound, the sample after acid treatment is washed with deionized for several times to washing lotion PH ≈ 7, filtering, finally by institute again
Obtain powder to dry under the conditions of 55 DEG C, this product is titanate radical nanopipe powder.
1.5g titanate radical nanopipes are dispersed in 50~80mL deionized water solutions, stirs and volume integral is added dropwise into solution
Number is 6~8% glacial acetic acid until the pH value of solution is 3~4, and 150mL silane coupling agents are being added after 1~2h is stirred at room temperature
KH550 ethanol solutions (V silane coupling agents:V ethanol ≈ 1:80) 3.5~5h, mistake, are then stirred under 75~85 DEG C of constant temperatures
Filter, deionized water wash for several times to washing lotion PH ≈ 7, dry, be subsequently placed in Muffle furnace at 500 DEG C under the conditions of 50~60 DEG C
Under the conditions of roast 1~2h, obtain earth silicon/titanic oxide composite nano tube.The above-mentioned composite nano tubes of 1g are finally weighed to disperse
In the sodium hydroxide solution that 50mL concentration is 1.5moL/L, 3~4h is stirred at room temperature, filters, deionized water is washed for several times
To washing lotion PH ≈ 7, dried under the conditions of 60 DEG C, that is, obtain high-temperature stable titania nanotube powder.Its scanning electron microscope (SEM) photograph, thoroughly
Electron microscope, X-ray diffractogram are penetrated respectively as shown in Fig. 5, Fig. 6, Fig. 7.From Fig. 5-6, titanium dioxide manufactured in the present embodiment
Nanotube dust can keep good tubular morphology under the calcination temperature higher than 400 DEG C.
Embodiment 3：
8g anatase titania nano powders are added in the sodium hydroxide solution that 180mL concentration is 10moL/L, stirring
And be transferred in reaction kettle, hydrothermal temperature is 120 DEG C, and the reaction time is 18~24h, naturally cools to room temperature.Filter, go
Ion water washing is for several times to washing lotion PH ≈ 7.Supernatant is removed, the hydrochloric acid solution of 0.1~0.5moL/L is added to above-mentioned powder
In, stirring or 2~3h of ultrasound, the sample after acid treatment is washed with deionized for several times to washing lotion PH ≈ 7 again, is filtered, most
Gained powder is dried under the conditions of 50~60 DEG C afterwards, this product is titanate radical nanopipe powder.
2g titanate radical nanopipes ultrasonic agitation is dispersed in 80mL deionized water solutions and forms solution A, by 1g cetyls
Trimethylammonium bromide is dissolved in 15mL deionized water solutions and forms solution B, 0.6mL ethyl orthosilicates are dissolved in 80~
Solution C is formed in 100mL ethanol solutions, solution B is slowly added dropwise in solution A and is vacuumized and is stirred under 0.08~0.1MPa
Mix 1.5~2h.Then solution C is slowly added dropwise to again, under normal pressure 1.5~2h of lower stirring, by 3mL ammonia spirit (ammonium hydroxide
Volume fraction is 15%) to be slowly added dropwise to stir 1.5~2h, filtering down under normal pressure into above-mentioned solution, and ethanol solution washs for several times,
Dried under the conditions of 50~60 DEG C, be subsequently placed in Muffle furnace 1~2h of roasting under the conditions of 550 DEG C, obtain silica/bis-
Titanium oxide composite nano tube.Finally weigh the above-mentioned composite nano tubes of 1g be dispersed in 50mL concentration be 1.5moL/L sodium hydroxide it is molten
In liquid, 3~4h is stirred at room temperature, filters, deionized water is washed for several times to washing lotion PH ≈ 7, is dried under the conditions of 50~60 DEG C,
Obtain high-temperature stable titania nanotube powder.Its scanning electron microscope (SEM) photograph, transmission electron microscope picture difference are as shown in Figure 8, Figure 9.By
Fig. 8-9 understands that titania nanotube powder manufactured in the present embodiment can keep good under the calcination temperature higher than 400 DEG C
Tubular morphology.
Claims (3)
1. a kind of high-temperature stable titania nanotube raw powder's production technology, it is characterised in that this method comprises the following steps：
1) titanic oxide nano is added in the sodium hydroxide solution of 9-15moL/L, 110~130 DEG C of stirrings are lower to carry out water
12~48h of thermal response, naturally cools to room temperature, it is 7 that filtering, deionized water, which are washed to washing lotion pH, by 0.1~0.5moL/L's
Hydrochloric acid solution is added in above-mentioned powder, stirring or 2~3h of ultrasound, and it is 7 to be washed with deionized again to washing lotion pH, filtering,
Finally gained powder is dried under the conditions of 50~60 DEG C and obtains titanate radical nanopipe；
2) surface modification, high-temperature roasting prepare earth silicon/titanic oxide composite nano tube powder, in following two methods
Any one：Method one：The titanate radical nanopipe that step 1) is obtained is dispersed in deionized water solution, is stirred and into solution
It is 5~8% glacial acetic acid until the pH values of solution are 3~4 that volume fraction, which is added dropwise, and silane idol is added after 1~2h is stirred at room temperature
Join agent ethanol solution, then stir 3.5~5h, filtering in 75~85 DEG C of constant temperature, it is 7 that deionized water, which is washed to washing lotion pH, 50
Dried under the conditions of~60 DEG C, be subsequently placed in Muffle furnace under the conditions of 425~550 DEG C and roast 1~2h, acquisition silica/
Titanium dioxide composite nano tube powder；The mass volume ratio of the titanate radical nanopipe and silane coupling agent ethanol solution for 0.5~
2g:30~150mL；The volume ratio of silane coupling agent and ethanol is 1 in the silane coupling agent ethanol solution:50~150；Method
Two：The titanate radical nanopipe ultrasonic agitation that step 1) obtains is dispersed in 80~100mL deionized water solutions and forms solution A, will
0.75-2 grams of cetyl trimethylammonium bromide is dissolved in 10~15mL deionized water solutions and forms solution B, by 0.6-2.5mL
Ethyl orthosilicate is dissolved in 80~100mL ethanol solutions and forms solution C, solution B is slowly added dropwise in solution A and
1.5~2h is stirred under 0.08~0.1MPa；Then solution C is slowly added dropwise to again, under normal pressure 1.5~2h of lower stirring, then
The ammonia spirit that 3~5mL volume fractions are 15~25% is slowly added dropwise into 1.5~2h of lower stirring, is filtered, second under normal pressure
Alcoholic solution washs, and is dried under the conditions of 50~60 DEG C, be subsequently placed in Muffle furnace under the conditions of 425~550 DEG C roasting 1~
2h, obtains earth silicon/titanic oxide composite nano tube powder；
3) it is 1~1.5moL/L's the earth silicon/titanic oxide composite nano tube powder that step 2) obtains to be dispersed in concentration
In sodium hydroxide solution, 3~4h, filtering are stirred at room temperature, it is 7 that deionized water, which is washed to washing lotion pH, is dried at 50~60 DEG C
It is dry, that is, obtain high-temperature stable titania nanotube powder.
2. high-temperature stable titania nanotube raw powder's production technology according to claim 1, it is characterised in that described
Silane coupling agent is selected from Si-69, KH550, KH560, KH570, more than one or both of KHA-171 or A-172.
3. high-temperature stable titania nanotube raw powder's production technology according to claim 1, it is characterised in that step
1) 6-8g anatase titania nano powders are added to 115-120 in the sodium hydroxide solution of 150~180mL 10moL/L in
DEG C stirring is lower carries out 18~36h of hydro-thermal reaction, naturally cools to room temperature, it is 7 that filtering, deionized water, which are washed to washing lotion pH, will
The hydrochloric acid solution of 0.1~0.5moL/L is added in above-mentioned powder, and stirring or 2~3h of ultrasound, are washed with deionized number again
It is secondary to washing lotion pH be 7, filtering, finally gained powder is dried under the conditions of 50~60 DEG C and obtains titanate radical nanopipe.
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