CN107381621A - A kind of preparation method of mesoporous indium oxide - Google Patents
A kind of preparation method of mesoporous indium oxide Download PDFInfo
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- CN107381621A CN107381621A CN201710424449.4A CN201710424449A CN107381621A CN 107381621 A CN107381621 A CN 107381621A CN 201710424449 A CN201710424449 A CN 201710424449A CN 107381621 A CN107381621 A CN 107381621A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The present invention relates to a kind of preparation method of mesoporous indium oxide, belongs to mesoporous materials field.The present invention prepares silica by raw material of quartz sand first, react to obtain sodium silicate solution with alkali again, then using pollen as template, pollen is impregnated in sodium silicate solution, the internal pollen with sodium silicate solution is calcined again, obtain mesoporous silicon oxide, impregnated again by template of mesoporous silicon oxide in nitric acid solution of indium, after calcining again, with alkali by silica dissolution, mesoporous indium oxide is can obtain, activation modification finally is carried out to mesoporous indium oxide with vapor and carbon dioxide, increases its specific surface area.Mesoporous indium oxide pore size prepared by the present invention is homogeneous, aperture system easy to control in size in preparation process.
Description
Technical field
The present invention relates to a kind of preparation method of mesoporous indium oxide, belongs to mesoporous materials field.
Background technology
People study the M41S series silicon-based mesoporous materials of synthesis, by the hole size range of ordering rule porous material from micro-
Hole extend to mesoporous；The SBA series silicon-based mesoporous material of synthesis is even more further to lift hole size range；Its high-sequential
Pore passage structure, huge specific surface area and pore volume, the unique physicochemical properties such as adjustable aperture so that this material
There is huge application potential in photoelectric device, separating-purifying, biomaterial, catalysis, advanced composite material (ACM) etc., in chemistry
The numerous areas such as engineering, information engineering, biotechnology, environmental energy have particularly important application value.
Mesoporous material research range gradually expands to non-silicon sill such as metal oxide from silicon-based mesoporous material.With silicon substrate
Mesoporous material is compared, non-silicon-based mesoporous material particularly metal oxide due to the diversity of its component and the polytropy of valence state,
Possess and be more widely applied scope.
Indium oxide is a kind of new n-type transparent semiconductor functional material, has wider energy gap, less resistivity
Higher catalytic activity, it is widely applied in terms of photoelectric field, gas sensor, catalyst.And indium oxide particles
When size reaches Nano grade in addition to function above, the skin effect, quantum size effect, small chi of nano material have been also equipped with
Very little effect and macro quanta tunnel effect etc., belong to one kind of mesoporous material.At present prepared by conventional soft template method, is specifically
By the use of surfactant as structure directing agent, self assembling process is completed using its interface interaction between species.It is but soft
The extremely difficult control of the hydrolysis of metal ion in template preparation process, the mesoporous material of every kind of metal oxide are required for different conjunctions
Into method, complicated reaction system and strict reaction condition, this greatly constrains non-silicon-based mesopore oxide material
The research work such as development and application, and pore size is difficult to control during preparing indium oxide, causes indium oxide aperture heterogeneity.
It would therefore be highly desirable to developing a kind of homogeneous indium oxide in aperture has necessary meaning.
The content of the invention
The technical problems to be solved by the invention：Pore size is difficult to control in being prepared for conventional oxidation indium, and aperture is not
A kind of the defects of homogeneous, there is provided preparation method of mesoporous indium oxide.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）100~200g quartz sands are crushed, sieving, quartz sand powder is obtained, by quartz sand powder, 400~500mL mass
Fraction filters after being 15% 40~50min of hydrochloric acid stirring reaction, silica is obtained, by silica and 200~300mL mass
Fraction is that 20% sodium hydroxide reacts 1~2h, obtains sodium silicate solution；
（2）It is 75% ethanol solution and 50~60mL by sodium silicate solution, 40~50g rape pollens, 80~100mL mass fractions
Mass fraction is 20% hydrochloric acid, is filtered after 60~90min of stirring reaction, obtains filter cake, filter cake is placed in Muffle furnace, and be passed through
Air, 2~3h is calcined at 500~600 DEG C, calcined product is obtained, calcined product is washed, obtain mesoporous silicon oxide；
（3）It is to be centrifuged after 45% indium nitrate mixes 2~3h by mesoporous silicon oxide and 200~300mL mass fractions, obtains
Sediment, put the precipitate in Muffle furnace, and be passed through air, 3~4h is calcined at 400~500 DEG C, by calcined product and
200~300mL mass fractions filter after being 25% 1~2h of sodium hydroxide solution stirring reaction, obtain filter residue, by filter residue and 100~
200mL mass fractions mix for 10% carbon acid solution, activate 2~3h at 300~400 DEG C, produce mesoporous indium oxide.
Step（2）Described in the speed that is passed through of air be 30~40mL/min.
Step（3）Described in the speed of centrifugation be 4000~5000r/min, centrifugation time is 5~10min.
Step（3）Described in activation when can also be passed through nitrogen, the speed that is passed through of nitrogen is 25~35mL/min.
Compared with other method, advantageous effects are the present invention：
The present invention can remove impurity using quartz sand as raw material after HCl treatment, obtain silica, then by silica and hydrogen
Sodium oxide molybdena is reacted to obtain sodium metasilicate, then using the rape pollen of porous stent structure as template, sodium metasilicate and hydrochloric acid reaction are obtained
Silicic acid, silicic acid are carried on pollen by gelation, then through calcining, obtain mesoporous silicon oxide, then using mesoporous silicon oxide as
Template, after loading indium nitrate, calcined in atmosphere, remove inner silica silicon with sodium hydroxide reaction, obtain mesoporous oxygen
Change indium, activation modification finally carried out to mesoporous indium oxide with vapor and carbon dioxide, increase its specific surface area, preparation it is mesoporous
Indium oxide pore size is homogeneous, and aperture is controlled effectively.
Embodiment
100~200g quartz sands are weighed first to be added in pulverizer after crushing, are crossed 80~100 mesh sieves, are obtained quartz sand
Powder, quartz sand powder is poured into and filled in the beaker that 400~500mL mass fractions are 15% hydrochloric acid solution, stirring reaction 40~
After 50min, filtering, silica is obtained, it is 20% sodium hydroxide that silica, which is added to, and fills 200~300mL mass fractions
In the beaker of solution, 1~2h of stirring reaction, obtain sodium silicate solution, weigh 40~50g rape pollens be added to fill 80~
100mL mass fractions is in the beaker of 75% ethanol solution, it are 20% salt to add sodium silicate solution and 50~60mL mass fractions
Acid, after 60~90min of stirring reaction, filtering, filter cake is obtained, and filter cake is placed in Muffle furnace, and be passed through air, be passed through speed
For 30~40mL/min, 500~600 DEG C are warming up to, it is 15~20 DEG C/min to control heating rate, insulation 2~3h of calcining, is obtained
Calcined product, and cleaned 3~5 times with water, mesoporous silicon oxide is obtained, mesoporous silicon oxide is added to and fills 200~300mL
Mass fraction is in the beaker of 45% nitric acid solution of indium, is poured into after 2~3h of immersion treatment in centrifuge, with 4000~5000r/
Min speed 5~10min of centrifugal treating, obtains sediment, puts the precipitate in baking oven after drying 40~50min and is transferred to
In Muffle furnace, and it is passed through air and 3~4h is calcined at 400~500 DEG C, calcining terminates, and the material after calcining is added to and filled
200~300mL mass fractions are in the beaker of 25% sodium hydroxide solution, after 1~2h of stirring reaction, filtering, obtain filter residue, and
Filter residue is added in activation furnace, it is 10% carbon acid solution to add 100~200mL mass fractions, and nitrogen is passed through into activation furnace
Gas, it is 25~35mL/min to control intake, is warming up to 300~400 DEG C of 2~3h of activation, and it is 10~15 DEG C to control heating rate,
End to be activated, obtains mesoporous indium oxide.
Example 1
100g quartz sands are weighed first to be added in pulverizer after crushing, are crossed 80 mesh sieves, quartz sand powder are obtained, by quartz sand powder
End, which is poured into, to be filled in the beaker that 400mL mass fractions are 15% hydrochloric acid solution, after stirring reaction 40min, filtering, obtains titanium dioxide
Silicon, silica is added to and filled in the beaker that 200mL mass fractions are 20% sodium hydroxide solution, stirring reaction 1h, is obtained
Sodium silicate solution, weigh 40g rape pollens be added to fill 80mL mass fractions be 75% ethanol solution beaker in, add
Sodium silicate solution and 50mL mass fractions are 20% hydrochloric acid, after stirring reaction 60min, filtering, obtain filter cake, and filter cake is placed in
In Muffle furnace, and air is passed through, it is 30mL/min to be passed through speed, is warming up to 500 DEG C, and it is 15 DEG C/min to control heating rate, is protected
Temperature calcining 2h, obtains calcined product, and is cleaned 3 times with water, obtains mesoporous silicon oxide, mesoporous silicon oxide is added to and filled
200mL mass fractions are in the beaker of 45% nitric acid solution of indium, are poured into after immersion treatment 2h in centrifuge, with 4000r/min's
Speed centrifugal treating 5min, obtains sediment, puts the precipitate in baking oven after drying 40min and is transferred in Muffle furnace, and leads to
Enter air and 3h is calcined at 400 DEG C, calcining terminates, and it is 25% hydrogen-oxygen that the material after calcining, which is added to, and fills 200mL mass fractions
In the beaker for changing sodium solution, after stirring reaction 1h, filtering, filter residue is obtained, and filter residue is added in activation furnace, added
100mL mass fractions are 10% carbon acid solution, and nitrogen is passed through into activation furnace, and it is 25mL/min to control intake, is warming up to
300 DEG C of activation 2h, it is 10 DEG C to control heating rate, end to be activated, obtains mesoporous indium oxide.
Mesoporous indium oxide aperture of the present invention is homogeneous, and particle diameter is 20~30nm, and traditional indium oxide particle diameter is 10~40nm.
Ordered mesoporous indium oxide prepared by the 0.3g present invention is weighed to be added in the flask for filling 100mL phenol solutions, with
The mode of bubbling is passed through air to drag, and it is 40mL/min to control air mass flow, while the ultraviolet light for being 254nm with wavelength
Irradiation.After testing, the use of degradation rate of the phenol of mesoporous indium oxide of the present invention in 1 hour is 55.2%, in 3 hours
Degradation rate is 72.1%.
Example 2
150g quartz sands are weighed first to be added in pulverizer after crushing, are crossed 90 mesh sieves, quartz sand powder are obtained, by quartz sand powder
End, which is poured into, to be filled in the beaker that 450mL mass fractions are 15% hydrochloric acid solution, after stirring reaction 45min, filtering, obtains titanium dioxide
Silicon, silica is added to and filled in the beaker that 250mL mass fractions are 20% sodium hydroxide solution, stirring reaction 2h, is obtained
Sodium silicate solution, weigh 45g rape pollens be added to fill 90mL mass fractions be 75% ethanol solution beaker in, add
Sodium silicate solution and 55mL mass fractions are 20% hydrochloric acid, after stirring reaction 75min, filtering, obtain filter cake, and filter cake is placed in
In Muffle furnace, and air is passed through, it is 35mL/min to be passed through speed, is warming up to 550 DEG C, and it is 18 DEG C/min to control heating rate, is protected
Temperature calcining 3h, obtains calcined product, and is cleaned 4 times with water, obtains mesoporous silicon oxide, mesoporous silicon oxide is added to and filled
250mL mass fractions are in the beaker of 45% nitric acid solution of indium, are poured into after immersion treatment 3h in centrifuge, with 4500r/min's
Speed centrifugal treating 8min, obtains sediment, puts the precipitate in baking oven after drying 45min and is transferred in Muffle furnace, and leads to
Enter air and 4h is calcined at 450 DEG C, calcining terminates, and it is 25% hydrogen-oxygen that the material after calcining, which is added to, and fills 250mL mass fractions
In the beaker for changing sodium solution, after stirring reaction 2h, filtering, filter residue is obtained, and filter residue is added in activation furnace, added
150mL mass fractions are 10% carbon acid solution, and nitrogen is passed through into activation furnace, and it is 30mL/min to control intake, is warming up to
350 DEG C of activation 3h, it is 13 DEG C to control heating rate, end to be activated, obtains mesoporous indium oxide.
Mesoporous indium oxide aperture of the present invention is homogeneous, and particle diameter is 20~30nm, and traditional indium oxide particle diameter is 10~40nm.
Ordered mesoporous indium oxide prepared by the 0.4g present invention is weighed to be added in the flask for filling 130mL phenol solutions, with
The mode of bubbling is passed through air to drag, and it is 40mL/min to control air mass flow, while the ultraviolet light for being 254nm with wavelength
Irradiation.After testing, the use of degradation rate of the phenol of mesoporous indium oxide of the present invention in 1 hour is 55.8%, in 3 hours
Degradation rate is 72.9%.
Example 3
200g quartz sands are weighed first to be added in pulverizer after crushing, are crossed 100 mesh sieves, quartz sand powder are obtained, by quartz sand
Powder, which pours into, to be filled in the beaker that 500mL mass fractions are 15% hydrochloric acid solution, after stirring reaction 50min, filtering, obtains dioxy
SiClx, silica is added to and filled in the beaker that 300mL mass fractions are 20% sodium hydroxide solution, stirring reaction 2h, is obtained
To sodium silicate solution, weigh 50g rape pollens and be added to and fill in the beaker that 100mL mass fractions are 75% ethanol solution, then add
Enter sodium silicate solution and 60mL mass fractions are 20% hydrochloric acid, after stirring reaction 90min, filtering, obtain filter cake, and filter cake is put
In Muffle furnace, and air is passed through, it is 40mL/min to be passed through speed, is warming up to 600 DEG C, and it is 20 DEG C/min to control heating rate,
Insulation calcining 3h, obtains calcined product, and is cleaned 5 times with water, obtains mesoporous silicon oxide, mesoporous silicon oxide is added into Sheng
In the beaker for having the nitric acid solution of indium that 300mL mass fractions are 45%, poured into after immersion treatment 3h in centrifuge, with 5000r/min
Speed centrifugal treating 10min, obtain sediment, put the precipitate in baking oven dry 50min after be transferred in Muffle furnace, and
It is passed through air and 4h is calcined at 500 DEG C, calcining terminates, and it is 25% hydrogen that the material after calcining, which is added to, and fills 300mL mass fractions
In the beaker of sodium hydroxide solution, after stirring reaction 2h, filtering, filter residue is obtained, and filter residue is added in activation furnace, added
200mL mass fractions are 10% carbon acid solution, and nitrogen is passed through into activation furnace, and it is 35mL/min to control intake, is warming up to
400 DEG C of activation 3h, it is 15 DEG C to control heating rate, end to be activated, obtains mesoporous indium oxide.
Mesoporous indium oxide aperture of the present invention is homogeneous, and particle diameter is 20~30nm, and traditional indium oxide particle diameter is 10~40nm.
Ordered mesoporous indium oxide prepared by the 0.5g present invention is weighed to be added in the flask for filling 150mL phenol solutions, with
The mode of bubbling is passed through air to drag, and it is 40mL/min to control air mass flow, while the ultraviolet light for being 254nm with wavelength
Irradiation.After testing, the use of degradation rate of the phenol of mesoporous indium oxide of the present invention in 1 hour is 56.7%, in 3 hours
Degradation rate is 73.8%.
Claims (4)
1. a kind of preparation method of mesoporous indium oxide, it is characterised in that specifically preparation process is：
（1）100~200g quartz sands are crushed, sieving, quartz sand powder is obtained, by quartz sand powder, 400~500mL mass
Fraction filters after being 15% 40~50min of hydrochloric acid stirring reaction, silica is obtained, by silica and 200~300mL mass
Fraction is that 20% sodium hydroxide reacts 1~2h, obtains sodium silicate solution；
（2）It is 75% ethanol solution and 50~60mL by sodium silicate solution, 40~50g rape pollens, 80~100mL mass fractions
Mass fraction is 20% hydrochloric acid, is filtered after 60~90min of stirring reaction, obtains filter cake, filter cake is placed in Muffle furnace, and be passed through
Air, 2~3h is calcined at 500~600 DEG C, calcined product is obtained, calcined product is washed, obtain mesoporous silicon oxide；
（3）It is to be centrifuged after 45% indium nitrate mixes 2~3h by mesoporous silicon oxide and 200~300mL mass fractions, obtains
Sediment, put the precipitate in Muffle furnace, and be passed through air, 3~4h is calcined at 400~500 DEG C, by calcined product and
200~300mL mass fractions filter after being 25% 1~2h of sodium hydroxide solution stirring reaction, obtain filter residue, by filter residue and 100~
200mL mass fractions mix for 10% carbon acid solution, activate 2~3h at 300~400 DEG C, produce mesoporous indium oxide.
A kind of 2. preparation method of mesoporous indium oxide according to claim 1, it is characterised in that step（2）Described in
The speed that is passed through of air is 30~40mL/min.
A kind of 3. preparation method of mesoporous indium oxide according to claim 1, it is characterised in that step（3）Described in
The speed of centrifugation is 4000~5000r/min, and centrifugation time is 5~10min.
A kind of 4. preparation method of mesoporous indium oxide according to claim 1, it is characterised in that step（3）Described in
Nitrogen can also be passed through during activation, the speed that is passed through of nitrogen is 25~35mL/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204818A (en) * | 2020-01-17 | 2020-05-29 | 山东大学 | Method for preparing magnetic mesoporous silica particles by using pollen as template |
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| CN102874823A (en) * | 2012-10-24 | 2013-01-16 | 南开大学 | Method for preparing silicon dioxide hollow microspheres with uniform shape by taking pollen grains as biological template |
| CN103910361A (en) * | 2014-03-10 | 2014-07-09 | 苏州科技学院相城研究院 | Method used for taking pollen and triblock copolymer as templates for synthesizing of mesoporous silica microspheres |
| CN106248747A (en) * | 2016-06-29 | 2016-12-21 | 燕园众欣纳米科技（北京）有限公司 | A kind of preparation method of Graphene mesoporous indium oxide nano composite material |
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2017
- 2017-06-07 CN CN201710424449.4A patent/CN107381621A/en active Pending
Patent Citations (4)
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| CN102795662A (en) * | 2012-08-29 | 2012-11-28 | 天津大学 | Method for preparing ordered mesoporous indium tin oxide material |
| CN102874823A (en) * | 2012-10-24 | 2013-01-16 | 南开大学 | Method for preparing silicon dioxide hollow microspheres with uniform shape by taking pollen grains as biological template |
| CN103910361A (en) * | 2014-03-10 | 2014-07-09 | 苏州科技学院相城研究院 | Method used for taking pollen and triblock copolymer as templates for synthesizing of mesoporous silica microspheres |
| CN106248747A (en) * | 2016-06-29 | 2016-12-21 | 燕园众欣纳米科技（北京）有限公司 | A kind of preparation method of Graphene mesoporous indium oxide nano composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204818A (en) * | 2020-01-17 | 2020-05-29 | 山东大学 | Method for preparing magnetic mesoporous silica particles by using pollen as template |
| CN111204818B (en) * | 2020-01-17 | 2021-10-26 | 山东大学 | Method for preparing magnetic mesoporous silica particles by using pollen as template |
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