CN101402463A - Process for producing transition metal oxide nano-slice - Google Patents
Process for producing transition metal oxide nano-slice Download PDFInfo
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- CN101402463A CN101402463A CNA2008102024698A CN200810202469A CN101402463A CN 101402463 A CN101402463 A CN 101402463A CN A2008102024698 A CNA2008102024698 A CN A2008102024698A CN 200810202469 A CN200810202469 A CN 200810202469A CN 101402463 A CN101402463 A CN 101402463A
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Abstract
The invention discloses a method for preparing a transition metal oxide nanometer sheet. A laminated compound of a transition metal salt is taken out and is poured to a grinding tank of a screw grinding machine; the grinding machine is started up and positively rotates for 1 to 5 minutes in order that the compound in the grinding tank is fully stirred; the grinding machine reversely rotates; the frequency is set between 30 and 45 Hz; the compound is ground for 6 to 18 hours; and the ground material is taken out, is added with n-tetrabutyl ammonium hydroxide or ethylenediamine according to the proportion of 0.4g/L and is subjected to centrifugation through a centrifuge at high speed of 10,000 revolutions/minute to obtain corresponding transparent sol of the transition metal oxide nanometer sheet. The method has simple operation, strong controllability and small energy consumption, saves time and raw materials, reduces cost, and is easy for large-scale production.
Description
Technical field
The present invention relates to a kind of lift-off technology of lamellar compound, specifically a kind of preparation method of transition metal oxide nano-slice.
Background technology
Lamellar compound is to pile up the space reticulated structure that forms by the elementary cell of certain ad hoc structure by shared angle, limit or face, is a kind of important solid functional materials.Because its distinctive laminate structure and interlayer chemical reactivity make it have broad application prospects at absorption, conduction, separation and catalytic field.Especially the research of semi-conductor stratiform compound causes people's extensive concern.And lamellar compound has a lot of modifying method as a kind of solid material, comprises physics, chemistry, machinery, chemical industry etc.In different research fields different research methods is arranged.The modifying method that wherein embeds and peel off is the good method that further prepares nanometer sheet.In the research of traditional stripping means, cardinal principle is to utilize similar and ethamine or 4-n-butyl ammonium hydroxide tensio-active agent, and lamellar compound is peeled off, and forms the colloidal sol of the stable transparent of nanometer sheet.Particle is very little, have plenty of individual layer and have plenty of multilayer, so this colloidal sol is very stable, can place a couple of days also be unlikely to the precipitation.Its concrete steps are: lamellar compound and 1M HCl are carried out ion-exchange, in order to make ion-exchange more completely, all will upgrade hydrochloric acid soln every day, probably through immersion-suction filtration-immersion revision test of 5-10 days, just can obtain protonated lamellar compound.This process has mainly been finished the ionic exchange, the more important thing is the increase of complete layer spacing, because hydrogen ion is with H when carrying out ion-exchange
3O
+Form react.Next step is the stripping process of protonated lamellar compound, utilize ethamine or 4-n-butyl ammonium hydroxide to insert and replace hydrogen ion as swelling agent, make interlamellar spacing further become big, thereby make the bonding force between the interlayer weaken, make and layer and layer slippage form very little individual layer or multiwalled nano-sheet material.
From then on since process was found, what people often at first considered was to come existing synthetic lamellar compound is peeled off with classical traditional test method.But, the lengthy and tedious complexity of this process, for a long time consuming time, often will pass through and just can obtain nano-film sol in tens of days, and the concentration of the colloidal sol of preparing is lower, controllability is relatively poor, and the needed expensive raw material price of pilot process, is not easy to large-scale production.
Summary of the invention
The preparation method of a kind of transition metal oxide nano-slice of providing at the deficiencies in the prior art is provided, and the nanometer sheet particle that this method obtains is less, and multilayer, single layer structure are arranged, and has good self-assembly performance; Its method is simple to operate, and energy consumption is little, saves time, and saves material, and cost is low, has the wide industrial prospect of production.
The object of the present invention is achieved like this:
A kind of preparation method of transition metal oxide nano-slice, it comprises following concrete steps:
A, get the lamellar compound of transition metal salt, be poured in the grinding pot of screw abrasive machine, open shredder, just changeing it was fully stirred in 1～5 minute in grinding pot;
B, counter-rotating shredder, and setpoint frequency 30～45HZ grind 6～18h;
Material after c, taking-up are ground with the ratio of 0.4g/L, adds 4-n-butyl ammonium hydroxide or quadrol, and is centrifugal under the supercentrifuge of 10000r/min, obtains corresponding transition metal oxide nano-slice vitreosol;
Wherein: transition metal salt comprises titanate, niobate, niobate-titanate, tantalate, tantalum titanate, manganate, wustite, cobaltates.
Screw abrasive machine of the present invention is disclosed " a kind of screw abrasive machine " Chinese invention patent application, application number: 200710170826.2.
The invention has the beneficial effects as follows:
(1), simple to operate, controllability is strong.
(2), save time.
(3), energy consumption is little, economize in raw materials, reduce cost.
(4), be easy to large-scale production.
Description of drawings
Fig. 1 is the XRD figure of the embodiment of the invention 6 gained lamellar compounds
Fig. 2 is the transmission electron microscope photo figure of the embodiment of the invention 5 gained colloidal sols
Fig. 3 is the transmission electron microscope photo figure of the embodiment of the invention 6 gained colloidal sols
Embodiment
Embodiment 1
A, with TiO
2With K
2CO
3With mol ratio is that 5.2: 1 mixed is even, is incubated 20h in 800 ℃ retort furnace, obtains the potassium titanate lamellar compound.
B, with excessive titanate stratiform compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 3 minutes, material is stirred in grinding pot fully, and definite add-on is 15g.
C, start shredder counter-rotating, setpoint frequency is 45HZ, begins to grind material violent phase mutual friction under this high speed shearing force.
After 9h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add the 100ml0.01mol/L 4-n-butyl ammonium hydroxide and carry out the peel separation experiment, centrifugal under the supercentrifuge of 10000r/min, obtain the titanium dioxide vitreosol.
F, the titanium dioxide vitreosol is carried out transmission electron microscope observing, can observe flaky material.
Embodiment 2
A, with Mn
2O
3With K
2CO
3With mol ratio is that 1: 1 mixed is even, is incubated 40h in 800 ℃ retort furnace, obtains the potassium manganate lamellar compound.
B, with excessive manganate lamellar compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 2 minutes, material is stirred in grinding pot fully, and definite add-on is 17g.
C, start shredder counter-rotating, setpoint frequency is 35Hz, begins to grind material violent phase mutual friction under this high speed shearing force.
After 11.5h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add the 100ml0.01mol/L 4-n-butyl ammonium hydroxide and carry out the peel separation experiment, centrifugal under the supercentrifuge of 10000r/min, obtain the Manganse Dioxide vitreosol.
F, Manganse Dioxide colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
Embodiment 3
A, with Nb2O5, TiO
2, K
2CO
3With mol ratio is that 1: 2: 1 mixed is even, is incubated 24h in 1100 ℃ retort furnace, obtains niobium potassium titanate lamellar compound.
B, with excessive niobium potassium titanate lamellar compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 4 minutes, material is stirred in grinding pot fully, and definite add-on is 24g.
C, start shredder counter-rotating, setpoint frequency is 30HZ, begins to grind material violent phase mutual friction under this high speed shearing force.
After 10h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add 100ml0.1mol/L ethamine and carry out the peel separation experiment.Centrifugal under the supercentrifuge of 10000r/min, obtain niobium titanium oxide transparent colloidal sol.
F, niobium titanium oxide colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
Embodiment 4
A, with Ta
2O
5, TiO
2, K
2CO
3With mol ratio is that 1: 2: 1 mixed is even, is incubated 24h in 1100 ℃ retort furnace, obtains tantalum titanium potassium acid lamellar compound.
B, with excessive tantalum titanate stratiform compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 3 minutes, material is stirred in grinding pot fully, and definite add-on is 26.7g.
C, start shredder counter-rotating, setpoint frequency is 40HZ, begins to grind material violent phase mutual friction under this high speed shearing force.
After d, grinding carry out 11.5, take out material.
E, get the 0.4g grinding material, add 100ml0.1mol/L ethamine and carry out the peel separation experiment, centrifugal under the supercentrifuge of 10000r/min, obtain tantalum titanium oxide transparent colloidal sol.
F, tantalum titanium oxide colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
Embodiment 5
A, with Nb
2O
5And K
2CO
3With mol ratio is that 1: 1 mixed is even, is incubated 24h in 1000 ℃ retort furnace, obtains potassium niobate stratiform compound.
B, with excessive potassium titanate lamellar compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 4 minutes, material is stirred in grinding pot fully, and definite add-on is 25g.
C, start shredder counter-rotating, setpoint frequency is 40HZ, begins to grind material violent phase mutual friction under this high speed shearing force.
After 6h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add the 100ml0.05mol/L 4-n-butyl ammonium hydroxide and carry out the peel separation experiment, centrifugal under the supercentrifuge of 10000r/min, obtain the niobium oxides vitreosol.
F, niobium oxides colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
Embodiment 6
A, with Nb
2O
5, TiO
2, K
2CO
3With mol ratio is that 2: 4: 1 mixed is even, is incubated 12h in 900 ℃ retort furnace, obtains niobium titanium potassium acid lamellar compound.
B, with excessive niobate-titanate lamellar compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 1 minute, material is stirred in grinding pot fully, and definite add-on is 22g.
C, start shredder counter-rotating, setpoint frequency 40HZ begins to grind, material violent phase mutual friction under this high speed shearing force.
After 18h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add the 100ml0.1mol/L quadrol and peel off, centrifugal under the supercentrifuge of 10000r/min, obtain niobium titanium oxide transparent colloidal sol.
F, niobium titanium oxide colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
Embodiment 7
A, with Na
2O
2, Co
3O
4With mol ratio is that 1: 1 mixed is even, is incubated 12h in 550 ℃ retort furnace, obtains cobalt acid sodium lamellar compound.
B, with excessive cobalt acid sodium lamellar compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 1 minute, material is stirred in grinding pot fully, and definite add-on is 19g.
C, start shredder counter-rotating, setpoint frequency 40HZ begins to grind, material violent phase mutual friction under this high speed shearing force.
After 9h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add the 100ml0.1mol/L 4-n-butyl ammonium hydroxide and peel off, centrifugal under the supercentrifuge of 10000r/min, obtain the cobalt oxide vitreosol.
F, cobalt oxide colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
A, with Na
2O
2, Fe
3O
4With mol ratio is that 1: 1 mixed is even, is incubated 14h in 550 ℃ retort furnace, obtains the sodium ferrite lamellar compound.
B, with excessive sodium ferrite lamellar compound, pour in the grinding pot of screw abrasive machine, open shredder, just changeing 5 minutes, material is stirred in grinding pot fully, and definite add-on is 19g.
C, start shredder counter-rotating, setpoint frequency 30HZ begins to grind, material violent phase mutual friction under this high speed shearing force.
After 9h is carried out in d, grinding, take out material.
E, get the 0.4g grinding material, add the 100ml0.1mol/L 4-n-butyl ammonium hydroxide and peel off, centrifugal under the supercentrifuge of 10000r/min, obtain the ferric oxide vitreosol.
F, ferric oxide colloidal sol is carried out transmission electron microscope observing, can observe flaky material.
Claims (1)
1, a kind of preparation method of transition metal oxide nano-slice is characterized in that it comprises following concrete steps:
A, get the lamellar compound of transition metal salt, be poured in the grinding pot of screw abrasive machine, open shredder, just changeing it was fully stirred in 1～5 minute in grinding pot;
B, counter-rotating shredder, and setpoint frequency 30～45HZ grind 6～18h;
Material after c, taking-up are ground with the ratio of 0.4g/L, adds 4-n-butyl ammonium hydroxide or quadrol, and is centrifugal under the supercentrifuge of 10000r/min, obtains corresponding transition metal oxide nano-slice vitreosol;
Wherein: transition metal salt comprises titanate, niobate, niobate-titanate, tantalate, tantalum titanate, manganate, wustite, cobaltates.
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|---|---|---|---|
| CN2008102024698A CN101402463B (en) | 2008-11-10 | 2008-11-10 | Process for producing transition metal oxide nano-slice |
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|---|---|---|---|
| CN2008102024698A CN101402463B (en) | 2008-11-10 | 2008-11-10 | Process for producing transition metal oxide nano-slice |
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| CN101402463B CN101402463B (en) | 2010-06-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811044A (en) * | 2010-04-23 | 2010-08-25 | 华东理工大学 | Potassium niobate nanotube photocatalyst and preparation method and application thereof |
| CN104852015A (en) * | 2015-02-11 | 2015-08-19 | 深圳新宙邦科技股份有限公司 | Niobium pentoxide nanosheet composite material, preparation method and application thereof |
| CN105056988A (en) * | 2015-08-09 | 2015-11-18 | 大连理工大学 | Binary niobate-based hydrodeoxygenation catalyst, preparation therefor and application thereof |
| CN110950386A (en) * | 2019-12-09 | 2020-04-03 | 北京大学 | Preparation method of transition metal sulfide nanosheet powder |
-
2008
- 2008-11-10 CN CN2008102024698A patent/CN101402463B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811044A (en) * | 2010-04-23 | 2010-08-25 | 华东理工大学 | Potassium niobate nanotube photocatalyst and preparation method and application thereof |
| CN101811044B (en) * | 2010-04-23 | 2012-07-04 | 华东理工大学 | Potassium niobate nanotube photocatalyst and preparation method and application thereof |
| CN104852015A (en) * | 2015-02-11 | 2015-08-19 | 深圳新宙邦科技股份有限公司 | Niobium pentoxide nanosheet composite material, preparation method and application thereof |
| CN105056988A (en) * | 2015-08-09 | 2015-11-18 | 大连理工大学 | Binary niobate-based hydrodeoxygenation catalyst, preparation therefor and application thereof |
| CN110950386A (en) * | 2019-12-09 | 2020-04-03 | 北京大学 | Preparation method of transition metal sulfide nanosheet powder |
| CN110950386B (en) * | 2019-12-09 | 2021-02-09 | 北京大学 | Preparation method of transition metal sulfide nanosheet powder |
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|---|---|
| CN101402463B (en) | 2010-06-02 |
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