CN108238632A - Titanyl cluster and its method that nano-titanium dioxide is prepared for magnanimity - Google Patents
Titanyl cluster and its method that nano-titanium dioxide is prepared for magnanimity Download PDFInfo
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- CN108238632A CN108238632A CN201611217494.4A CN201611217494A CN108238632A CN 108238632 A CN108238632 A CN 108238632A CN 201611217494 A CN201611217494 A CN 201611217494A CN 108238632 A CN108238632 A CN 108238632A
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Abstract
The present invention provides titanyl cluster and its method that nano-titanium dioxide is prepared for magnanimity, and in particular to titanyl cluster and its method that nano-titanium dioxide is prepared for magnanimity.The present invention can be raw material by metal titanium salt and acid, and different titanyl cluster presomas is prepared using volatility process or solvent-thermal process method.Required titanyl cluster presoma can be selected to roast to obtain required nano-titanium dioxide as needed, and the preparation efficiency with high photocatalysis effect titanium dioxide can be significantly improved.Titanium dioxide prepared by the present invention has larger specific surface area and preferable pattern, can preferably apply in fields such as photocatalytic cleavage water, photocatalysis organic pollutant degradation, solar cells.
Description
Technical field
It is prepared the invention belongs to nano material and catalyst for preparing hydrogen technical field, and in particular to titanyl cluster and its for macro
The method that amount prepares nano-titanium dioxide.
Background technology
Since early 20th century, the commercialization preparation of titanium dioxide starts, and titanium dioxide is widely used in pigment, coating, tooth
Cream, suncream etc..1972, Teng Dao and Honda found that titanium dioxide as electrode, has light under the irradiation of ultraviolet light for the first time
The effect of water is catalytically decomposed.Since then, a large amount of scientists are dedicated to the research of titanic oxide material, photoelectricity, photocatalysis,
Also gradually prosperity is got up for the application in the fields such as sensing.
Usually there are three types of crystal forms for titanium dioxide, are anatase, rutile and brockite respectively.And golden red in these three crystal forms
Stone is stable phase, and anatase is metastable phase, and brockite is unstable phase, their stability is related to crystallite dimension.Due to
The size of grain has a series of advantages much smaller than ordinary titanium powder, nano-titanium dioxide：Skin effect, small-size effect and macroscopic view
Quantum tunneling effect etc..These effects are heavily dependent on the size, form and structure of its particle, so special needed for preparing
It is sized, the technology of the nano-titanium dioxide of form and structure seems particularly critical.The preparation method of nano-titanium dioxide at present
Mainly have：Sol-gal process, micella/reverse micelle method, hydrothermal/solvent method, direct oxidation method, chemical vapour deposition technique, ultrasound, from
The methods of assembling.However, these methods still need to constantly improve, and titanium dioxide is also required to improve as the performance of catalyst.
Invention content
The present invention provides a kind of preparation method of nano-titanium dioxide, including using titanyl cluster as presoma, roasting is made
Standby nano-titanium dioxide.
According to the present invention, the temperature of the roasting can be selected from 400 to 800 DEG C, preferably 450 to 600 DEG C, for example, 500 to
550℃。
According to the present invention it is possible to different calcination temperatures is selected to prepare different-shape and the dioxy of specific surface area as needed
Change titanium.
According to the present invention it is possible to required titanyl cluster is selected to roast the titanium dioxide for preparing different catalytic performances as needed
Titanium.
According to the present invention, the titanyl cluster (also known as " titanium cluster ") can be selected from titanium sulfate cluster, titanium benzoate cluster or it is mixed
Close object.
The present invention also provides a kind of preparation method of the titanyl cluster, including, for raw material, being used with metal titanium salt and acid
The titanyl cluster is prepared in volatility process or solvent-thermal process method.
According to the present invention, the metal titanium salt can be selected from metal-organic titanium salt, such as isopropyl titanate, the positive fourth of metatitanic acid
Ester, cyclopentadienyl titanium dichloride or its mixture.
Acid of the present invention can be inorganic acid or organic acid.The acid is not particularly limited in the present invention, example
Such as, inorganic acid can be selected from one or more in hydrochloric acid, hydrobromic acid, hydroiodic acid, sulfuric acid, pyrosulfuric acid, phosphoric acid, nitric acid；It is organic
Acid can be selected from formic acid, acetic acid, acetoacetate, pyruvic acid, trifluoroacetic acid, propionic acid, butyric acid, caproic acid, enanthic acid, hendecanoic acid, the moon
It is one or more in cinnamic acid, benzoic acid, salicylic acid.Embodiment according to the present invention, the acid can be with its anhydrous shapes
Formula or the form of aqueous solution use.As example, can use one or more in concentrated hydrochloric acid, the concentrated sulfuric acid, concentrated nitric acid.
The molar ratio of the metal titanium salt and acid can be 1:1 to 1:100, such as 1:15 to 1:100.
According to the present invention, the preparation method of the titanyl cluster can carry out in a solvent.The solvent can be selected from water
(such as distilled water) or organic solvent.Wherein, organic solvent is not particularly limited, as long as it may be adapted to carry out solvent-thermal process
Method.Preferably, the solvent is the solvent inert to reaction reagent.As illustrative example, organic solvent can be with
Selected from nitrile solvents (such as acetonitrile), aromatic hydrocarbon solvent (such as benzene, toluene), alcohols solvent (such as methanol, ethyl alcohol, isopropanol, positive third
Alcohol), ether solvent (such as ether), esters solvent (such as ethyl acetate), in halogenated hydrocarbon solvent (such as dichloromethane, carbon tetrachloride)
It is one or more.
The molar ratio of the solvent and metal titanium salt can be 500:1 to 1:1, preferably 5:1 to 2:1.
The preparation of the titanyl cluster can carry out in the presence of organic base template.Do not have for organic base template
It is particularly limited to, as long as it may be adapted to carry out titanium cluster synthesis.As example, piperazine, triethylene diamine, divinyl can be selected from
It is one or more in triamine, hexamethylenetetramine.
The molar ratio of the organic base template and metal titanium salt can be 3:1 to 1:4, preferably 2:1 to 1:1.
As example, the titanium sulfate cluster can be prepared for example, by following method：
Distilled water is measured, adds in 98% concentrated sulfuric acid, piperazine is added with stirring, tetrabutyl titanate is added dropwise after to be dissolved；
Continue stirring to clarify completely to solution, stand volatilization or rotated using revolving instrument, treat the volatilization of most of water or
After steaming, beaker sealing is placed in the refrigerator not higher than 5 DEG C and is cooled down, is preferably cooled down 1 hour or more, such as 5 hours, you can obtain sulphur
Sour titanium cluster.
As another example, the titanium benzoate cluster can be prepared for example, by following method：
Benzoic acid is weighed, is dissolved in spare in acetonitrile；
It measures isopropyl titanate to be placed in reaction kettle, adds in acetonitrile dissolving；
The benzoic acid solution dissolved before is added in reaction kettle, is put into baking oven and heats 10 hours or more, such as 15 hours,
Obtain titanium benzoate cluster.
Preferably, it after obtaining the titanium cluster, is also filtered and dry.
The present invention also provides the titanyl clusters that such as described preparation method is prepared.
The present invention also provides the titanium dioxide that such as described preparation method is prepared.The titanium dioxide can be used for photocatalysis
The fields such as splitting water, photocatalysis organic pollutant degradation, solar cell；Preferably, the titanium dioxide splits for photocatalysis
Xie Shui prepares hydrogen.
Advantageous effect
The present invention can be raw material by metal titanium salt and acid, and difference is prepared using volatility process or solvent-thermal process method
Titanyl cluster presoma.According to the present invention, titanium dioxide prepared by the present invention, which has, reaches as high as 4527 μm of olh-1·g-1
Catalysis hydrogen-producing speed.Also, it using the method for the present invention, can be adjusted according to titanium dioxide to the different demands of catalytic performance
Whole titanyl cluster or adjustment calcination temperature as raw material, to prepare the titanium dioxide of different catalytic performances, and can be notable
Improve the preparation efficiency with photocatalysis effect titanium dioxide.
Titanium dioxide prepared by the present invention has larger specific surface area and preferable pattern, can preferably apply in light
The fields such as catalytic pyrolysis water, photocatalysis organic pollutant degradation, solar cell.
Description of the drawings：
Fig. 1：The scanning electron microscope (SEM) photograph of titanium dioxide that titanium sulfate cluster is obtained as 500~800 DEG C of roastings of presoma；
Fig. 2：The scanning electron microscope (SEM) photograph of titanium dioxide that titanium benzoate cluster is obtained as 500~800 DEG C of roastings of presoma；
Fig. 3：Titanium sulfate cluster X-ray powder diffraction figure, wherein the line of lower section is theoretical value, the line of top is experiment value；
Fig. 4：Titanium benzoate cluster X-ray powder diffraction figure, wherein the line of lower section is theoretical value, the line of top is experiment value；
Fig. 5：The X-ray powder diffraction figure of titanium dioxide that different titanium cluster presomas are roasted in different temperatures.Wherein
Each label collection of illustrative plates meaning is as follows：
a：The TiO that titanium sulfate cluster is obtained as 500 DEG C of roastings of presoma2；
b：The TiO that titanium benzoate cluster is obtained as 500 DEG C of roastings of presoma2；
c：The TiO that titanium sulfate cluster is obtained as 600 DEG C of roastings of presoma2；
d：The TiO that titanium benzoate cluster is obtained as 600 DEG C of roastings of presoma2；
e：The TiO that titanium sulfate cluster is obtained as 700 DEG C of roastings of presoma2；
f：The TiO that titanium benzoate cluster is obtained as 700 DEG C of roastings of presoma2；
g：The TiO that titanium sulfate cluster is obtained as 800 DEG C of roastings of presoma2；
h：The TiO that titanium benzoate cluster is obtained as 800 DEG C of roastings of presoma2。
Fig. 6：The infared spectrum of titanium dioxide that titanium sulfate cluster is obtained as 500~800 DEG C of roastings of presoma, wherein collection of illustrative plates
It is respectively from top to bottom 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C of collection of illustrative plates
Fig. 7：The infared spectrum of titanium dioxide that titanium benzoate cluster is obtained as 500~800 DEG C of roastings of presoma, wherein by
Up to it is lower be respectively 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C of collection of illustrative plates；
Fig. 8：The uv-spectrogram of titanium dioxide that titanium sulfate cluster is obtained as 500~800 DEG C of roastings of presoma, wherein by upper
To it is lower be respectively 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C of collection of illustrative plates；
Fig. 9：The uv-spectrogram of titanium dioxide that titanium benzoate cluster is obtained as 500~800 DEG C of roastings of presoma, wherein by
Up to it is lower be respectively 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C of collection of illustrative plates；
Figure 10：The hydrogen output figure for the titanium dioxide that different titanium cluster presomas are roasted in different temperatures.Wherein each mark
Remember that collection of illustrative plates meaning is as follows：
a：The TiO that titanium sulfate cluster is obtained as 500 DEG C of roastings of presoma2；
b：The TiO that titanium benzoate cluster is obtained as 500 DEG C of roastings of presoma2；
c：The TiO that titanium sulfate cluster is obtained as 600 DEG C of roastings of presoma2；
d：The TiO that titanium benzoate cluster is obtained as 600 DEG C of roastings of presoma2；
e：The TiO that titanium sulfate cluster is obtained as 700 DEG C of roastings of presoma2；
f：The TiO that titanium benzoate cluster is obtained as 700 DEG C of roastings of presoma2；
g：The TiO that titanium sulfate cluster is obtained as 800 DEG C of roastings of presoma2；
h：The TiO that titanium benzoate cluster is obtained as 800 DEG C of roastings of presoma2。
Specific embodiment
Technical scheme of the present invention is described in detail below by way of illustrative specific embodiment, but should not be by these
Embodiment is construed to limiting the scope of the invention.All technologies realized based on the above of the present invention are encompassed by this
Invention is intended in the range of protection.
Unless otherwise indicated, the raw materials and reagents used in embodiment are commercial materials.
The powder diagram of titanium dioxide is characterized with MiniFlex II powder diffractometers.
Titanium dioxide infared spectrum is characterized with VERTEX70.
Titanium dioxide uv-spectrogram is characterized with PerkinElmer Lambda 35.
Titanium dioxide scanning electron microscope (SEM) photograph is characterized with JSM-6700.
Titanium dioxide hydrogen output is tested with Labsolar hydrogen generating systems.
Preparation of the 1. titanium sulfate cluster of embodiment as the titanium dioxide of presoma
10 milliliters of distilled water are measured in beaker, add in 3.05 gram of 98% concentrated sulfuric acid, stirring adds in 0.178 gram in stirring
0.687 gram of tetrabutyl titanate is added dropwise after to be dissolved in organic base template piperazine.Continue stirring to clarify completely to solution, standing is waved
Hair is rotated using revolving instrument, after most of water volatilizees or steams, beaker sealing is placed in 5 DEG C of refrigerator and cools down 5
Hour, you can colourless column titanium sulfate cluster (being determined by X-ray powder diffraction) is obtained, obtained titanium sulfate cluster is filtered, it is dry,
It is placed in crucible, is put into Muffle furnace and 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C of calcination temperature is set and is roasted 12 hours, you can
Required titanium dioxide.The scanning electron microscope of the titanium dioxide is illustrated in Fig. 1, and X-ray powder diffraction figure is shown in Fig. 5, the results showed that
500 DEG C, 600 DEG C of obtained titanium dioxide be Anatase, 700 DEG C of obtained titanium dioxide are Anatase, Rutile Type
Mixed phase, 800 DEG C of obtained titanium dioxide are Rutile Types.
Preparation of the 2. titanium benzoate cluster of embodiment as the titanium dioxide of presoma
1.13 grams of benzoic acid are weighed, are dissolved in 10 milliliters of acetonitriles, 0.3 milliliter of isopropyl titanate is measured and is placed in polytetrafluoroethylene (PTFE)
In reaction kettle, 1 milliliter of acetonitrile dissolving is added in, the benzoic acid solution dissolved before is added in reaction kettle, is put into 100 DEG C of baking ovens
Heating 15 hours, cooling, obtains faint yellow needle-shaped titanium benzoate cluster crystal body (being determined by X-ray powder diffraction).By what is obtained
Titanium benzoate cluster filters, dry, is placed in crucible, be put into Muffle furnace set 500 DEG C of calcination temperature, 600 DEG C, 700 DEG C, 800
DEG C and roast 12 hours, you can needed for titanium dioxide.The scanning electron microscope of the titanium dioxide is illustrated in Fig. 2, and x-ray powder spreads out
It penetrates and is illustrated in Fig. 5, the results showed that 500 DEG C of obtained titanium dioxide are Anatases, and 600 DEG C of obtained titanium dioxide are anatases
Phase, the mixed phase of Rutile Type, 700 DEG C, 800 DEG C of obtained titanium dioxide be Rutile Type.
The hydrogen yield test of 3. Titanium Dioxide of embodiment
The method of the present invention can obtain different-shape, structure, catalysis using different titanyl cluster presomas as needed
The titanium dioxide of efficiency.
In the present embodiment, using the titanium dioxide test hydrogen yield obtained in Examples 1 and 2, specific test condition
It is as follows with parameter：
90 ml deionized waters, 10 ml methanols are added in into reaction kettle, 40 milligrams of samples add in 33 microlitres with liquid-transfering gun
Chloroplatinic acid, covers reaction kettle, is evacuated in liquid with vacuum pump no longer generates bubble while stirring, (complete using 300W xenon lamps
Wave band) irradiation.Sampling is primary per hour, samples four times, records peak area, calculates hydrogen output and hydrogen-producing speed.
1. titanium dioxide sample hydrogen-producing speed of table summarizes with specific surface area
Wherein each sample symbol meaning is as follows：
a：The TiO that titanium sulfate cluster is obtained as 500 DEG C of roastings of presoma2；
b：The TiO that titanium benzoate cluster is obtained as 500 DEG C of roastings of presoma2；
c：The TiO that titanium sulfate cluster is obtained as 600 DEG C of roastings of presoma2；
d：The TiO that titanium benzoate cluster is obtained as 600 DEG C of roastings of presoma2；
e：The TiO that titanium sulfate cluster is obtained as 700 DEG C of roastings of presoma2；
f：The TiO that titanium benzoate cluster is obtained as 700 DEG C of roastings of presoma2；
g：The TiO that titanium sulfate cluster is obtained as 800 DEG C of roastings of presoma2；
h：The TiO that titanium benzoate cluster is obtained as 800 DEG C of roastings of presoma2。
Exemplary illustration has been carried out to embodiments of the present invention above.But the present invention is not limited to above-mentioned embodiment party
Formula.All within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done, should be included in the present invention
Protection domain within.
Claims (10)
1. a kind of preparation method of nano-titanium dioxide, including using titanyl cluster as presoma, roasting prepares nanometer titanium dioxide
Titanium.
2. the preparation method of nano-titanium dioxide as described in claim 1, wherein：The temperature of the roasting can be selected from 400
To 800 DEG C, preferably 450 to 600 DEG C, such as 500 to 550 DEG C；
Preferably, different calcination temperatures can be selected to prepare different-shape and the titanium dioxide of specific surface area as needed；
Preferably, the titanyl cluster can be selected from titanium sulfate cluster, titanium benzoate cluster or its mixture.
3. a kind of preparation method of titanyl cluster as claimed in claim 1 or 2, including, for raw material, being adopted with metal titanium salt and acid
It is prepared with volatility process or solvent-thermal process method.
4. a kind of preparation method of titanyl cluster as claimed in claim 3, wherein：The metal titanium salt can have selected from metal
Machine titanium salt；
Preferably, the acid can be inorganic acid or organic acid；
Preferably, the preparation of the titanyl cluster can carry out in a solvent；
Preferably, the preparation of the titanyl cluster can carry out in the presence of organic base template.
5. a kind of preparation method of the titanyl cluster as described in claim 3 or 4, wherein：The metal titanium salt can be selected from metatitanic acid
It is one or more in isopropyl ester, tetrabutyl titanate, cyclopentadienyl titanium dichloride；
Inorganic acid can be selected from one or more in hydrochloric acid, hydrobromic acid, hydroiodic acid, sulfuric acid, pyrosulfuric acid, phosphoric acid, nitric acid；It is organic
Acid can be selected from formic acid, acetic acid, acetoacetate, pyruvic acid, trifluoroacetic acid, propionic acid, butyric acid, caproic acid, enanthic acid, hendecanoic acid, the moon
One or more acid in cinnamic acid, benzoic acid, salicylic acid can be used in the form of its anhydrous form or aqueous solution, example
Such as, it can use one or more in concentrated hydrochloric acid, the concentrated sulfuric acid, concentrated nitric acid；
The molar ratio of the metal titanium salt and acid can be 1:1 to 1:100, such as 1:15 to 1:100；
The solvent can be selected from water or organic solvent, solvent preferably inert to reaction reagent, for example, organic solvent can be with
One kind or more in nitrile solvents, aromatic hydrocarbon solvent, alcohols solvent, ether solvent, esters solvent, halogenated hydrocarbon solvent
Kind；
The molar ratio of the solvent and metal titanium salt can be 500:1 to 1:1, preferably 5:1 to 2:1；
The organic base template can be selected from one kind in piperazine, triethylene diamine, diethylenetriamine, hexamethylenetetramine or more
Kind；
The molar ratio of the organic base template and metal titanium salt can be 3:1 to 1:4, preferably 2:1 to 1:1.
6. the preparation method of titanyl cluster as described in claim any one of 3-5, wherein：
It can be prepared via a method which titanium sulfate cluster：
Distilled water is measured, adds in 98% concentrated sulfuric acid, piperazine is added with stirring, tetrabutyl titanate is added dropwise after to be dissolved；
Continue stirring to clarify completely to solution, stand volatilization or rotated using revolving instrument, treat most of water volatilization or steam
Afterwards, beaker sealing is placed in the refrigerator not higher than 5 DEG C and cooled down, preferably cooled down 1 hour or more, such as 5 hours, you can obtain titanium sulfate
Cluster；
Alternatively, it can be prepared via a method which titanium benzoate cluster：
Benzoic acid is weighed, is dissolved in spare in acetonitrile；
It measures isopropyl titanate to be placed in reaction kettle, adds in acetonitrile dissolving；
The benzoic acid solution dissolved before is added in reaction kettle, is put into baking oven and heats 10 hours or more, such as 15 hours, is obtained
Titanium benzoate cluster；
Preferably, it after obtaining the titanium cluster, is also filtered and dry.
7. the titanyl cluster obtained such as any one of claim 3-6 preparation methods.
8. the titanium dioxide that the preparation method as described in right 1 or 2 obtains.
9. titanium dioxide according to any one of claims 8 is for photocatalytic cleavage water, photocatalysis organic pollutant degradation, solar cell
The purposes in the fields of grade.
10. the purposes described in claim 9, wherein the titanium dioxide prepares hydrogen for photocatalytic cleavage water.
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| CN110734458A (en) * | 2018-07-19 | 2020-01-31 | 中国科学院福建物质结构研究所 | Macro preparation method of titanium oxide clusters |
| CN110975852A (en) * | 2019-12-24 | 2020-04-10 | 济南大学 | Titanium dioxide nanocluster @ carbon sphere multilevel composite structure material and preparation method and application thereof |
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| CN114907419A (en) * | 2022-05-18 | 2022-08-16 | 山东交通学院 | Silver-titanium dissimilar metal cluster compound and room temperature macroscopic quantity synthesis method thereof |
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