CN104140123B - A kind of three-dimensional flower-shaped metatitanic acid material of being assembled by laminar nano sheet and synthetic method thereof - Google Patents
A kind of three-dimensional flower-shaped metatitanic acid material of being assembled by laminar nano sheet and synthetic method thereof Download PDFInfo
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- CN104140123B CN104140123B CN201410350522.4A CN201410350522A CN104140123B CN 104140123 B CN104140123 B CN 104140123B CN 201410350522 A CN201410350522 A CN 201410350522A CN 104140123 B CN104140123 B CN 104140123B
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Abstract
The invention discloses a kind of three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet, assembled by the nanometer sheet of outwards dispersing from structure centre, the length of laminar nano sheet is 100-600nm, thickness is the number of plies of each laminar nano sheet of 10-15nm is 6-10 layer, and the interlamellar spacing of laminar nano sheet is 0.5-1.5nm; Also disclosing the synthetic method of this three-dimensional flower-shaped metatitanic acid material, take TBT as silicon source, and acetic acid is solvent, and P123, as stablizer, is titanium source with tetra-n-butyl titanate, is synthesized by solvent thermal reaction.Synthetic method of the present invention is simple, does not need to rely on raw-material crystal formation and size, and product structure is stablized, and productive rate is high, is uniformly dispersed.
Description
Technical field
The present invention relates to a kind of three-dimensional flower-shaped metatitanic acid material of being assembled by laminar nano sheet and synthetic method thereof, belong to field of material synthesis technology.
Background technology
Lamellar compound, due to the laminate structure of its uniqueness, is not only many chemical reactions and provides microreactor, simultaneously can as the elementary cell of other materials.Layered titanic acid is a kind of important n-type semi-conductor, belongs to TiO
2derivative, in nature with TiO
2similar and be all semiconductor material.Metatitanic acid nanometer sheet has typical two-dirnentional structure, derives from the delamination of lamellar precursor, therefore maintain precursor rhombic form structure, and laminate is with the feature of negative charge.Because of the physics of its uniqueness, chemistry and optical property, studied application widely, comprised opto-electronic conversion, magneto-optic effect, high-k device, moisture sensor, photochemical catalysis, automatically cleaning, and the field such as biosensor.More importantly layered titanic acid has the characteristics such as regular laminate structure, interlayer ion exchange and the swelling stripping of laminate, by expanding its range of application to its longitudinal doping vario-property.Therefore, the application of layered titanic acid in opto-electronic conversion and photochemical catalysis more and more causes the attention of people.The three-dimensional flower-shaped structure be assembled into by two-dimensional nano sheet has high surface area, high reaction activity etc. and is better than the nano metal of other shapes and the character of nano metal compound-material, as flower-like structure Cu
2s has very high photocatalytic activity (CrystEngComm, 2011,13,6549), CuO nano flower film has super-hydrophobicity (Electrochim.Acta, 2007,57,951), CuO/Ni flower-like structure film is applied to the electrochemical activity (Electrochim.Acta that electrode improves electrode, 2009,54,1161).In addition, some nano metal particles have serious reunion and particle arch formation in actual applications, thus limit the performance of its nano effect and the large advantage of specific surface area, and these agglomerations can be avoided after controlling synthesis flower-like structure and still there is the good advantage of the nano effect structural stability of nano particle.Therefore three-dimensional flower-shaped structure is studied application widely.
In recent years, the preparation method of metatitanic acid has high temperature solid-state method, hydrothermal synthesis method, sol-gel method, organic precursor method, and wherein high temperature solid-state method and hydrothermal method are the most conventional.High temperature solid-state method obtains metatitanic acid by high-temperature calcination, but the poor controllability of this method, structure is easily caved in, and easily reunites (J.Am.Ceram.Soc., 1998,71, C-49).Water heat transfer mainly utilizes hydro-thermal reaction, in alkali, process TiO
2the metatitanic acid (Catal.Commun., 2009,10,378) obtained.These two kinds of methods all depend on precursor TiO
2crystal formation and size, these methods are not generally had specific morphology simultaneously, size differs, the nanoparticle that impurity is more, these are all unfavorable for the transmission of photogenerated charge and are separated, thus cause the right compound of electronics and hole, have impact on the catalytic performance of material, limit the Synthesis and application of metatitanic acid.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide a kind of three-dimensional flower-shaped metatitanic acid material of being assembled by laminar nano sheet and synthetic method thereof, take tetra-n-butyl titanate as titanium source, synthesized the metatitanic acid of the three-dimensional flower-shaped structure be self-assembled into by two-dimensional layer nanometer sheet by solvent thermal reaction.Synthetic method is simple, does not need to rely on raw-material crystal formation and size, and product structure is stablized, and productive rate is high, is uniformly dispersed.
For achieving the above object, the present invention adopts following technical scheme:
A kind of three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet, described three-dimensional flower-shaped metatitanic acid is assembled by the laminar nano sheet outwards dispersed from structure centre, the length of laminar nano sheet is 100-600nm, width is 50-200nm, thickness is 10-15nm, the number of plies of each laminar nano sheet is 6-10 layer, and the interlamellar spacing of laminar nano sheet is 0.5-1.5nm.Preferably, the interlamellar spacing of laminar nano sheet is 0.83nm.
The synthetic method of this three-dimensional flower-shaped metatitanic acid material, comprises the following steps:
(1) in polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer (P123), add acetic acid, be warming up to 30-50 DEG C, stirring and dissolving;
(2) in the solution of step (1), add tetrabutyl titanate (TBT), stop after stirring and dissolving stirring, obtain white " milky " thing, leave standstill sustained reaction 2-96h;
(3) move in reactor by reacted for step (2) white " milky " thing, 130-180 DEG C of standing 20-28h, obtains white precipitate;
(4) white precipitate is separated, washing, dry, obtain the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet.
Wherein, in step (1), (2), the ratio of the add-on of P123, acetic acid, tetrabutyl titanate is 1g:(30-40) mL:(0.5-2.5) mL.
In step (4), white precipitate adopts centrifugation or suction filtration to be separated; Washing adopts alcohol flushing; Drying temperature is 60-100 DEG C, and time of drying is 18-30h.
Preferably, in step (1), (2), the ratio of the add-on of P123, acetic acid, tetrabutyl titanate is 1g:36.75mL:1.0mL.
Preferably, in step (2), leaving standstill the sustained reaction time is 24-96h.
The application of three-dimensional flower-shaped metatitanic acid material in the fields such as opto-electronic conversion, magneto-optic effect, high-k device, moisture sensor, photochemical catalysis, automatically cleaning and biosensor that the present invention obtains.
Beneficial effect of the present invention:
(1) the present invention take TBT as silicon source, acetic acid is solvent, P123 is as stablizer, synthesize the three-dimensional flower-shaped metatitanic acid assembled by laminar nano sheet, wherein can regulate the length of stratiform nanometer sheet by changing time of repose, not needing to rely on raw-material crystal formation and size, product structure is stablized, productive rate is high, is uniformly dispersed;
(2) simple, with low cost, the synthetic method mild condition of synthetic method, has higher commercial applications prospect.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the flower-shaped metatitanic acid assembled by laminar nano sheet that the embodiment of the present invention 1 prepares;
Fig. 2 be the embodiment of the present invention 1 prepare be flower-shaped metatitanic acid laminate nanometer sheet HRTEM figure;
Fig. 3 is the SEM figure of the flower-shaped metatitanic acid assembled by laminar nano sheet that the embodiment of the present invention 2 prepares.
Fig. 4 is the TEM figure of the flower-shaped metatitanic acid assembled by laminar nano sheet that the embodiment of the present invention 2 prepares.
Fig. 5 is the SEM that the embodiment of the present invention 3 prepares the flower-shaped metatitanic acid assembled by laminar nano sheet.
Fig. 6 is the HRTEM figure that the embodiment of the present invention 3 prepares flower-shaped metatitanic acid laminate nanometer sheet, and its interlamellar spacing is 0.83nm, and the number of plies is 6-10 layer.
Fig. 7 is the XRD figure of the flower-shaped metatitanic acid of embodiment of the present invention 1-3 gained.
Embodiment
The present invention is further illustrated in conjunction with the embodiments, should be noted that following explanation is only to explain the present invention, not limiting its content.
Embodiment 1
1.00g P123 is added in the beaker of 100mL, beaker is placed on magnetic stirring apparatus, add 36.75mL acetic acid and be warming up to 40 DEG C, be stirred to and dissolve completely.The TBT of 1.00mL is added in beaker, stops after stirring and dissolving stirring, obtain white " milky " thing.Above-mentioned milk is left standstill sustained reaction 2h, the white " milky " thing solution obtained is gone in 50mL reactor, be placed in 150 DEG C of thermostat containers and leave standstill 24h.By white precipitate solution suction filtration after cooling, with ethanol filtration washing repeatedly, the white sample throw out dry 24h at 60 DEG C obtained, obtain the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet, productive rate is 30%.
Fig. 1 is the SEM figure of three-dimensional flower-shaped metatitanic acid material prepared by the present embodiment, Fig. 2 is the HRTEM figure of the three-dimensional flower-shaped metatitanic acid laminate nanometer sheet that the embodiment of the present invention prepares, as can be seen from Fig. 1 and Fig. 2, flower-shaped metatitanic acid is assembled by laminar nano sheet, the length of laminar nano sheet is about 100nm, and the interlamellar spacing of laminar nano sheet is 0.83nm.By controlling the flower-shaped metatitanic acid of synthesis, the phenomenons such as the serious agglomeration that metatitanic acid not only can be avoided to exist in actual applications and particle bridge formation, and still maintain the nano effect structure of nano particle, the advantage of good stability.
Embodiment 2:
1.00g P123 is added in the beaker of 100mL, beaker is placed on magnetic stirring apparatus, add 36.75mL acetic acid and be warming up to 40 DEG C, be stirred to and dissolve completely.The TBT of 1.00mL is added in beaker, stops after stirring and dissolving stirring, obtain white " milky " thing.Above-mentioned milk is left standstill sustained reaction 24h, the white " milky " thing solution obtained is gone in 50mL reactor, be placed in 150 DEG C of thermostat containers and leave standstill 24h.By white precipitate solution suction filtration after cooling, with ethanol filtration washing repeatedly, the white sample throw out dry 24h at 60 DEG C obtained, obtain the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet, productive rate is 28%.
Fig. 3 is the SEM figure of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet prepared by the present embodiment, the TEM figure of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet that Fig. 4 is prepared for the present embodiment, as seen from Figure 3, the length being assembled into the laminar nano sheet of flower-shaped metatitanic acid is about 200-500nm; As seen from Figure 4, three-dimensional flower-shaped structure has the outside divergent structure in center, good dispersity.
Embodiment 3:
1.00g P123 is added in the beaker of 100mL, beaker is placed on magnetic stirring apparatus, add 36.75mL acetic acid and be warming up to 40 DEG C, be stirred to and dissolve completely.The TBT of 1.00mL is added in beaker, stops after stirring and dissolving stirring, obtain white " milky " thing.Above-mentioned milk is left standstill sustained reaction 96h, the white " milky " thing solution obtained is gone in 50mL reactor, be placed in 150 DEG C of thermostat containers and leave standstill 24h.By white precipitate solution suction filtration after cooling, with ethanol filtration washing repeatedly, the white sample throw out dry 24h at 60 DEG C obtained, obtain the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet, productive rate is 35%.
Fig. 5 is the SEM figure of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet prepared by the present embodiment, the HRTEM figure of Fig. 6 flower-shaped metatitanic acid laminate nanometer sheet for the present embodiment prepares, as seen from Figure 5, the length being assembled into the laminar nano sheet of flower-shaped metatitanic acid is about 400-700nm; As seen from Figure 6, the number of plies of laminar nano sheet is 6-10 layer, and interlamellar spacing is 0.83nm.
Fig. 7 is the XRD figure of the flower-shaped metatitanic acid of embodiment of the present invention 1-3 gained, and its diffraction peak is typical metatitanic acid structure as seen from the figure, and flower-shaped metatitanic acid must interlamellar spacing be 1-1.3nm.
Embodiment 4
1.00g P123 is added in the beaker of 100mL, beaker is placed on magnetic stirring apparatus, add 30mL acetic acid and be warming up to 30 DEG C, be stirred to and dissolve completely.The TBT of 0.5mL is added in beaker, stops after stirring and dissolving stirring, obtain white " milky " thing.Above-mentioned milk is left standstill sustained reaction 48h, the white " milky " thing solution obtained is gone in 50mL reactor, be placed in 130 DEG C of thermostat containers and leave standstill 28h.By white precipitate solution suction filtration after cooling, with ethanol filtration washing repeatedly, the white sample throw out dry 18h at 100 DEG C obtained, obtain the three-dimensional flower-shaped metatitanic acid material of the laminar nano sheet assembling being about 300-400nm by length, productive rate is 30%.
Embodiment 5
1.00g P123 is added in the beaker of 100mL, beaker is placed on magnetic stirring apparatus, add 40mL acetic acid and be warming up to 30 DEG C, be stirred to and dissolve completely.The TBT of 2.5mL is added in beaker, stops after stirring and dissolving stirring, obtain white " milky " thing.Above-mentioned milk is left standstill sustained reaction 48h, the white " milky " thing solution obtained is gone in 50mL reactor, be placed in 180 DEG C of thermostat containers and leave standstill 20h.By white precipitate solution suction filtration after cooling, with ethanol filtration washing repeatedly, the white sample throw out dry 18h at 100 DEG C obtained, obtain the three-dimensional flower-shaped metatitanic acid material of the laminar nano sheet assembling being about 400-600nm by length, productive rate is 33%.
Under visible light, the three-dimensional flower-shaped metatitanic acid material that the present invention obtains can be used for taking paper waste as the photochemical catalysis of target degradation product.
Claims (10)
1. the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet, it is characterized in that, described three-dimensional flower-shaped metatitanic acid is assembled by the nanometer sheet of outwards dispersing from structure centre, the length of laminar nano sheet is 100-600nm, width is 50-200nm, thickness is 10-15nm, and the number of plies of each laminar nano sheet is 6-10 layer, and the interlamellar spacing of laminar nano sheet is 0.5-1.5nm;
This three-dimensional flower-shaped metatitanic acid material is by by adding acetic acid in P123, is warming up to 30-50 DEG C, stirring and dissolving, then adds tetrabutyl titanate, stops stirring, obtains white " milky " thing, leave standstill sustained reaction 2-96h after stirring and dissolving; Move in reactor by reacted white " milky " thing, 130-180 DEG C of standing 20-28h, obtains white precipitate, is separated by white precipitate, washing, dry and obtain;
The ratio of the add-on of P123, acetic acid, tetrabutyl titanate is 1g:(30-40) mL:(0.5-2) mL.
2. a kind of three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 1, it is characterized in that, the interlamellar spacing of laminar nano sheet is 0.83nm.
3. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet described in claim 1 or 2, is characterized in that, comprise the following steps:
(1) in P123, add acetic acid, be warming up to 30-50 DEG C, stirring and dissolving;
(2) in the solution of step (1), add tetrabutyl titanate, stop after stirring and dissolving stirring, obtain white " milky " thing, leave standstill sustained reaction 2-96h;
(3) move in reactor by reacted for step (2) white " milky " thing, 130-180 DEG C of standing 20-28h, obtains white precipitate;
(4) white precipitate is separated, washing, dry, obtain the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet;
Wherein, in step (1), (2), the ratio of the add-on of P123, acetic acid, tetrabutyl titanate is 1g:(30-40) mL:(0.5-2) mL.
4. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 3, is characterized in that, in step (4), white precipitate adopts centrifugation or suction filtration to be separated; Washing adopts alcohol flushing; Drying temperature is 60-100 DEG C, and time of drying is 18-30h.
5. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 3, it is characterized in that, in step (1), (2), the ratio of the add-on of P123, acetic acid, tetrabutyl titanate is 1g:36.75mL:1.0mL.
6. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 3, is characterized in that, in step (2), leaving standstill the sustained reaction time is 24-96h.
7. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 3, is characterized in that, comprise the following steps: in 1.00g P123, add 36.75mL acetic acid be warming up to 40 DEG C, be stirred to and dissolve completely; Add the TBT of 1.00mL again, stop after stirring and dissolving stirring, obtain white " milky " thing; Above-mentioned milk is left standstill sustained reaction 2h, reacted white " milky " thing solution is gone in reactor, be placed in 150 DEG C of thermostat containers and leave standstill 24h; Be separated by white precipitate solution suction filtration after cooling, with ethanol filtration washing throw out repeatedly, at 60 DEG C, dry 24h, to obtain final product.
8. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 3, is characterized in that, comprise the following steps: in 1.00g P123, add 36.75mL acetic acid be warming up to 40 DEG C, be stirred to and dissolve completely; Add the TBT of 1.00mL again, stop after stirring and dissolving stirring, obtain white " milky " thing; Above-mentioned milk is left standstill sustained reaction 24h, reacted white " milky " thing solution is gone in reactor, be placed in 150 DEG C of thermostat containers and leave standstill 24h; Be separated by white precipitate solution suction filtration after cooling, with ethanol filtration washing throw out repeatedly, at 60 DEG C, dry 24h, to obtain final product.
9. the synthetic method of the three-dimensional flower-shaped metatitanic acid material assembled by laminar nano sheet as claimed in claim 3, is characterized in that, comprise the following steps: in 1.00g P123, add 36.75mL acetic acid be warming up to 40 DEG C, be stirred to and dissolve completely; Add the TBT of 1.00mL again, stop after stirring and dissolving stirring, obtain white " milky " thing; Above-mentioned milk is left standstill sustained reaction 96h, reacted white " milky " thing solution is gone in reactor, be placed in 150 DEG C of thermostat containers and leave standstill 24h; Be separated by white precipitate solution suction filtration after cooling, with ethanol filtration washing throw out repeatedly, at 60 DEG C, dry 24h, to obtain final product.
10. the application of three-dimensional flower-shaped metatitanic acid material in opto-electronic conversion, magneto-optic effect, high-k device, moisture sensor, photochemical catalysis, automatically cleaning and bio-sensing field of being assembled by laminar nano sheet described in claim 1 or 2.
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