CN106542574A - The method of controlledly synthesis difference crystalline phase floriform appearance titanic oxide material - Google Patents
The method of controlledly synthesis difference crystalline phase floriform appearance titanic oxide material Download PDFInfo
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- CN106542574A CN106542574A CN201610947068.XA CN201610947068A CN106542574A CN 106542574 A CN106542574 A CN 106542574A CN 201610947068 A CN201610947068 A CN 201610947068A CN 106542574 A CN106542574 A CN 106542574A
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- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a kind of method of controlledly synthesis difference crystalline phase floriform appearance titanic oxide material，0.9～1.6g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols、In the mixed solvent of 0.25～1.8g Tetramethylammonium hydroxide and 1.1～1.8mL deionized waters，By 1.5～2.1mL template polystyrene sphere PS after being uniformly mixed、0.1g template poly(ethylene oxide) poly(propylene oxide) poly(ethylene oxide) triblock copolymer P123s or 0.3～0.5g template diallyl dimethyl ammoniumchlorides PDADMAC are added in above-mentioned system，Stir to fully dissolving，Then above-mentioned solution is transferred in hydrothermal reaction kettle in 180～200 DEG C of crystallizations，After the completion of reaction，The floriform appearance titanic oxide material with anatase crystal or brockite crystal formation is obtained by being dried after the solution sucking filtration after crystallization naturally.Preparation process is simple of the present invention, controllability are strong, and target product purity is high and favorable reproducibility, and obtained product morphology is novel.
Description
Technical field
The invention belongs to the synthesis technical field of titanic oxide material, and in particular to a kind of controlledly synthesis difference crystalline phase is flower-shaped
The method of pattern titanic oxide material.
Background technology
From Fujishima and Honda in 1972 deliver on Nature magazines with regard to TiO2Electrode glazing decomposition water
Since paper, due to its stable performance, photocatalytic activity it is high, nontoxic and with low cost etc., it is considered to be it is a kind of preferably
Conductor photocatalysis material, causes in fields such as solaode, photocatalytic pollutant degradations widely studied.Titanium dioxide is deposited
In three kinds of crystal formations：Rutile-type, Detitanium-ore-type and brookite type.Which has been obtained for various shapes in the range of micro-nano-scale
Looks such as nanometer rods, nano wire, nanometer sheet, nanotube and micro-nano ball etc..Scientific researcher shows through numerous studies, TiO2's
Microscopic appearance and crystal structure have directly impact to its catalysis activity and selectivity.Therefore, synthesis is with special microcosmic shape
The titanium dioxide micro-nano material of looks, it is considered to be one of effective way of regulation and control catalysis material activity.
Flower-shaped titanium dioxide is due to larger specific surface area, good light absorbs and refractive index, contributing to photoproduction load
The absorption of the sub generation of stream, migration and reactant on surface, reduces the compound probability of photoelectricity, more excellent so as to show
Photocatalytic activity.At present, despite the anatase with regard to preparing floriform appearance, the relevant report of brookite type titanium dioxide, but
There are still pattern single, step is complicated（Many one-step hydrothermals or high temperature and high pressure method）, the shortcomings of poor reproducibility.And adopt a step water
Full-boiled process, is capable of achieving controllable synthesis purity by the pH value and temperature of simple adjustment and control system higher, different floriform appearances
There is not been reported for anatase and brookite type titanium dioxide material.
The content of the invention
Present invention solves the technical problem that there is provided that a kind of preparation process is simple, controllability be strong and favorable reproducibility it is controllable
The method of the different crystalline phase floriform appearance titanic oxide materials of synthesis.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, controlledly synthesis difference crystalline phase floriform appearance dioxy
The method for changing titanium material, it is characterised in that concretely comprise the following steps：0.9～1.6g titanium tetraisopropylate TTIP are added to into 1.2mL isopropyls
In the mixed solvent of alcohol, 0.25～1.8g Tetramethylammonium hydroxide and 1.1～1.8mL deionized waters, will after being uniformly mixed
1.5～2.1mL template polystyrene sphere PS, 0.1g template poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three is embedding
Section copolymer p 123 or 0.3～0.5g template diallyl dimethyl ammoniumchlorides PDADMAC are added in above-mentioned system, are stirred
Mix to fully dissolving, then above-mentioned solution be transferred in hydrothermal reaction kettle in 180～200 DEG C of crystallizations, after the completion of reaction,
The floriform appearance titanium dioxide with anatase crystal or brockite crystal formation is obtained by being dried after the solution sucking filtration after crystallization naturally
Material.
Further preferably, the building-up process of the anatase titanium dioxide material with floriform appearance is：By 1.2～1.6g
Titanium tetraisopropylate TTIP is added to 1.2mL isopropanols, 0.25～0.4g Tetramethylammonium hydroxide and 1.1～1.3mL deionized waters
Mixed solvent in, 1.5～2.1mL template polystyrene sphere PS are added in above-mentioned system after being uniformly mixed,
Stir to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, will
Naturally dry after solution sucking filtration after crystallization and obtain the anatase titanium dioxide material with floriform appearance.
Further preferably, the concrete building-up process of the brookite type titanium dioxide material with Fructus Cucurbitae moschatae floriform appearance is：Will
0.9～1.6g titanium tetraisopropylate TTIP are added to 1.2mL isopropanols, 1.2～1.8g Tetramethylammonium hydroxide and 1.3～2.1mL
In the mixed solvent of deionized water, by 0.1g template poly(ethylene oxide)-poly(propylene oxide)-polycyclic oxygen second after being uniformly mixed
Alkane triblock copolymer P123 is added in above-mentioned system, is stirred to fully dissolving, above-mentioned solution is transferred to hydro-thermal then anti-
Answer in kettle in 180-200 DEG C of crystallization, after the completion of reaction, obtain being dried after the solution sucking filtration after crystallization naturally with Fructus Cucurbitae moschatae
The brookite type titanium dioxide material of floriform appearance.
Further preferably, the concrete building-up process of the brookite type titanium dioxide material with flying saucer floriform appearance is：Will
0.9～1.5g titanium tetraisopropylate TTIP are added to 1.2mL isopropanols, 0.8～1.3g Tetramethylammonium hydroxide and 1.2～1.8mL
In the mixed solvent of deionized water, 0.3～0.5g diallyl dimethyl ammoniumchlorides PDADMAC are added after being uniformly mixed
Enter in above-mentioned system, stir to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle anti-in 180 DEG C of crystallization
Should, after the completion of reaction, the brookite type dioxy with flying saucer floriform appearance is obtained by being dried after the solution sucking filtration after crystallization naturally
Change titanium material.
The present invention has advantages below：Preparation process is simple, controllability are strong, and target product purity is high and favorable reproducibility, institute
Obtained product morphology is novel, has broad application prospects in fields such as catalyst, lithium ion battery and photolysis water hydrogen manufacturing.
Description of the drawings
Fig. 1 is the XRD figure of the 1 obtained anatase titanium dioxide material with floriform appearance of embodiment；
Fig. 2 is the SEM figures of the 2 obtained anatase titanium dioxide material with floriform appearance of embodiment；
Fig. 3 is the XRD figure of the 4 obtained brookite type titanium dioxide material with Fructus Cucurbitae moschatae floriform appearance of embodiment；
Fig. 4 is the SEM figures of the 5 obtained brookite type titanium dioxide material with Fructus Cucurbitae moschatae floriform appearance of embodiment；
Fig. 5 is the SEM figures of the 7 obtained brookite type titanium dioxide material with flying saucer floriform appearance of embodiment.
Specific embodiment
By the following examples the above of the present invention is described in further details, but this should not be interpreted as this
The scope for inventing above-mentioned theme is only limitted to below example, and all technologies realized based on the above of the present invention belong to this
Bright scope.
Embodiment 1
1.6g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 0.4g Tetramethylammonium hydroxide and 1.3mL deionized waters
In mixed solvent, 2.1mL template polystyrene sphere PS are added in above-mentioned system after being uniformly mixed, are stirred to filling
Divide dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, after crystallization
Naturally dry after solution sucking filtration and obtain the anatase titanium dioxide material with floriform appearance.
1 XRD figure can be seen that obtained final products are anatase titanium dioxide with reference to the accompanying drawings, and have fine
Degree of crystallinity.
Embodiment 2
1.2g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 0.25g Tetramethylammonium hydroxide and 1.1mL deionized waters
Mixed solvent in, 1.5mL template polystyrene sphere PS are added in above-mentioned system after being uniformly mixed, stir to
Fully dissolve, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, after crystallization
Solution sucking filtration after dry naturally the anatase titanium dioxide material obtained with floriform appearance.
2 SEM figures are it can be seen that obtained final products are with the flower-like structure being made up of nanometer rods with reference to the accompanying drawings.
Embodiment 3
1.6g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 1.8g Tetramethylammonium hydroxide and 2.1mL deionized waters
In mixed solvent, after being uniformly mixed by 0.1g template poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three block altogether
Polymers P123 is added in above-mentioned system, stirs to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 200
DEG C crystallization, after the completion of reaction, obtains the plate titanium with Fructus Cucurbitae moschatae floriform appearance by being dried after the solution sucking filtration after crystallization naturally
Ore deposit type titanic oxide material.
Embodiment 4
1.3g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 1.5g Tetramethylammonium hydroxide and 1.8mL deionized waters
In mixed solvent, by 0.1g poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymers after being uniformly mixed
P123 is added in above-mentioned system, is stirred to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle brilliant in 200 DEG C
Change reaction, after the completion of reaction, the brookite type with Fructus Cucurbitae moschatae floriform appearance is obtained by being dried after the solution sucking filtration after crystallization naturally
Titanic oxide material.
3 XRD figure can be seen that obtained final products are brookite type titanium dioxide with reference to the accompanying drawings, and have fine
Degree of crystallinity.
Embodiment 5
0.9g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 1.2g Tetramethylammonium hydroxide and 1.3mL deionized waters
In mixed solvent, by 0.1g poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymers after being uniformly mixed
P123 is added in above-mentioned system, is stirred to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle brilliant in 180 DEG C
Change reaction, after the completion of reaction, the brookite type with Fructus Cucurbitae moschatae floriform appearance is obtained by being dried after the solution sucking filtration after crystallization naturally
Titanic oxide material.
4 SEM figures are it can be seen that obtained final products are with the Fructus Cucurbitae moschatae flower-like structure being made up of nanometer sheet with reference to the accompanying drawings.
Embodiment 6
1.5g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 1.3g Tetramethylammonium hydroxide and 1.8mL deionized waters
In mixed solvent, 0.5g diallyl dimethyl ammoniumchlorides PDADMAC are added in above-mentioned system after being uniformly mixed,
Stir to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, will
Naturally dry after solution sucking filtration after crystallization and obtain the brookite type titanium dioxide material with flying saucer floriform appearance.
Embodiment 7
1.1g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 0.8g Tetramethylammonium hydroxide and 1.2mL deionized waters
In mixed solvent, 0.3g diallyl dimethyl ammoniumchlorides PDADMAC are added in above-mentioned system after being uniformly mixed,
Stir to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, will
Naturally dry after solution sucking filtration after crystallization and obtain the brookite type titanium dioxide material with flying saucer floriform appearance.
5 SEM figures are it can be seen that obtained final products are with the flying saucer flower being made up of fish scale-shaped nanometer sheet with reference to the accompanying drawings
Shape structure.
Embodiment 8
0.9g titanium tetraisopropylate TTIP are added to into 1.2mL isopropanols, 0.8g Tetramethylammonium hydroxide and 1.2mL deionized waters
In mixed solvent, 0.3g diallyl dimethyl ammoniumchlorides PDADMAC are added in above-mentioned system after being uniformly mixed,
Stir to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, will
Naturally dry after solution sucking filtration after crystallization and obtain the brookite type titanium dioxide material with flying saucer floriform appearance.
Ultimate principle, principal character and the advantage of the present invention is embodiment above describes, the technical staff of the industry should
Understand, the present invention is not restricted to the described embodiments, the original for simply illustrating the present invention described in above-described embodiment and description
Reason, under the scope without departing from the principle of the invention, the present invention also has various changes and modifications, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (4)
1. the method for controlledly synthesis difference crystalline phase floriform appearance titanic oxide material, it is characterised in that concretely comprise the following steps：By 0.9～
1.6g titanium tetraisopropylate TTIP be added to 1.2mL isopropanols, 0.25～1.8g Tetramethylammonium hydroxide and 1.1～1.8mL go from
In the mixed solvent of sub- water, 1.5～2.1mL template polystyrene sphere PS, 0.1g template is gathered after being uniformly mixed
Oxide-polypropylene oxide-poly(ethylene oxide) triblock copolymer P123 or 0.3～0.5g template polydiene dimethylamines
Ammonium chloride PDADMAC is added in above-mentioned system, stirs to fully dissolving, above-mentioned solution is transferred to hydrothermal reaction kettle then
In in 180～200 DEG C of crystallizations, after the completion of reaction, obtain being dried after the solution sucking filtration after crystallization naturally with anatase
The floriform appearance titanic oxide material of crystal formation or brockite crystal formation.
2. the method for controlledly synthesis according to claim 1 difference crystalline phase floriform appearance titanic oxide material, its feature exist
In the building-up process of the anatase titanium dioxide material with floriform appearance it is：1.2～1.6g titanium tetraisopropylate TTIP are added
Enter in the mixed solvent of 1.2mL isopropanols, 0.25～0.4g Tetramethylammonium hydroxide and 1.1～1.3mL deionized waters, stir
1.5～2.1mL template polystyrene sphere PS are added in above-mentioned system after mix homogeneously, are stirred to fully dissolving, so
Afterwards above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, after the solution sucking filtration after crystallization
Naturally dry and obtain the anatase titanium dioxide material with floriform appearance.
3. the method for controlledly synthesis according to claim 1 difference crystalline phase floriform appearance titanic oxide material, its feature exist
In the concrete building-up process of the brookite type titanium dioxide material with Fructus Cucurbitae moschatae floriform appearance it is：By 0.9～1.6g, tetra- isopropanols
Titanium TTIP is added to the mixed solvent of 1.2mL isopropanols, 1.2～1.8g Tetramethylammonium hydroxide and 1.3～2.1mL deionized waters
In, by 0.1g template poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer P123 after being uniformly mixed
It is added in above-mentioned system, stirs to fully dissolving, then above-mentioned solution is transferred to brilliant in 180-200 DEG C in hydrothermal reaction kettle
Change reaction, after the completion of reaction, the brookite type with Fructus Cucurbitae moschatae floriform appearance is obtained by being dried after the solution sucking filtration after crystallization naturally
Titanic oxide material.
4. the method for controlledly synthesis according to claim 1 difference crystalline phase floriform appearance titanic oxide material, its feature exist
In the concrete building-up process of the brookite type titanium dioxide material with flying saucer floriform appearance it is：By 0.9～1.5g, tetra- isopropanols
Titanium TTIP is added to the mixed solvent of 1.2mL isopropanols, 0.8～1.3g Tetramethylammonium hydroxide and 1.2～1.8mL deionized waters
In, 0.3～0.5g diallyl dimethyl ammoniumchlorides PDADMAC are added in above-mentioned system after being uniformly mixed, are stirred
Mix to fully dissolving, then above-mentioned solution is transferred in hydrothermal reaction kettle in 180 DEG C of crystallizations, after the completion of reaction, by crystalline substance
Naturally dry after solution sucking filtration after change and obtain the brookite type titanium dioxide material with flying saucer floriform appearance.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101481140A (en) * | 2009-02-27 | 2009-07-15 | 上海师范大学 | Preparation of multi-level flower-like structure titanium dioxide |
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| CN103771505A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Synthetic method of titanium dioxide self-assembled particles |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481140A (en) * | 2009-02-27 | 2009-07-15 | 上海师范大学 | Preparation of multi-level flower-like structure titanium dioxide |
| KR20110061328A (en) * | 2009-12-01 | 2011-06-09 | (주) 그라비티 | Method for providing of game service and server thereof |
| GB2489007A (en) * | 2011-03-15 | 2012-09-19 | Secr Defence | A process for producing nanoparticles |
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