CN109626423A - A method of preparing poriferous titanium dioxide ball - Google Patents
A method of preparing poriferous titanium dioxide ball Download PDFInfo
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- CN109626423A CN109626423A CN201811545342.6A CN201811545342A CN109626423A CN 109626423 A CN109626423 A CN 109626423A CN 201811545342 A CN201811545342 A CN 201811545342A CN 109626423 A CN109626423 A CN 109626423A
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- titanium dioxide
- ball
- fluosite
- aminophenyl
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention relates to a kind of methods for preparing poriferous titanium dioxide ball, the following steps are included: 1) titanium dioxide precursor is added in the dispersion liquid of m-aminophenyl fluosite ball, it is centrifugated after stirring a few hours, obtains m-aminophenyl fluosite ball/titanium dioxide precursor compound；2) it by the resulting m-aminophenyl fluosite ball/titanium dioxide precursor compound of step 1), is put into standing in baking oven and is heat-treated for a period of time；3) m-aminophenyl fluosite ball/titanium dioxide precursor compound through Overheating Treatment is put into high temperature cabonization in a nitrogen atmosphere, and further roasting removes carbon elimination to get poriferous titanium dioxide ball in air；Compared with the existing technology, the preparation method is simply mild by the present invention, can adjust the size of titanium dioxide pore volume by changing the concentration of titanium dioxide precursor, and low in cost, the period is shorter, and yield is higher.
Description
[technical field]
The invention belongs to technical field of material, specifically a kind of method for preparing poriferous titanium dioxide ball.
[background technique]
Titanium dioxide is a kind of semiconductor photoelectrocatalysielectrode material cheap, safety is good, performance is stable, is had good
Photoelectricity, dielectric properties, and obtained extensively in the fields such as sensor, coating, the depollution of environment and photoelectrocatalysis, catalyst carrier
Application.
There are many kinds of titanium dioxide patterns, and different-shape influences the different physical and chemical properties of sample.Wherein, spherical more
Porous titanium dioxide material has lower density, high-specific surface area and good electron capture ability etc., causes that people's is more
Concern.Currently, patent and hollow titanium dioxide ball preparation method reported in the literature mainly use template agent method, that is, utilize micro-nano
The organic or inorganic material of rice does template, prepares in conjunction with the technologies such as electrochemical process, microemulsion polymerization method or colloidal sol, gel, will
Titanium dioxide precursor and template are assembled into core shell compound, then remove template, obtain corresponding hollow microsphere.Institute
Common hard mould agent includes polystyrene microsphere, Nano particles of silicon dioxide, soft template such as micella, lotion etc..
For hollow titanium dioxide ball, porous titanium dioxide ball, because containing porous inside ball, to have
There are bigger pore volume and higher specific surface area, more active materials can be adsorbed, and in catalytic field by bigger
Application.However, being reported in terms of the preparation of porous spherical titanium dioxide at present less.
[summary of the invention]
A kind of method for preparing poriferous titanium dioxide ball is provided present invention aim to solve above-mentioned deficiency, it should
Preparation method is simply mild, can adjust the size of titanium dioxide pore volume by changing the concentration of titanium dioxide precursor,
And it is low in cost, the period is shorter.
A kind of method for preparing poriferous titanium dioxide ball is designed to achieve the above object, comprising the following steps: 1) by dioxy
Change titanium precursor to be added in the dispersion liquid of m-aminophenyl fluosite ball, is centrifugated after stirring a few hours, obtains ammonia
Base phenol formaldehyde resin ball/titanium dioxide precursor compound；2) by resulting m-aminophenyl fluosite ball/bis- of step 1)
Titanium oxide precursor compound is put into standing in baking oven and is heat-treated for a period of time；3) by the m-aminophenyl through Overheating Treatment
Fluosite ball/titanium dioxide precursor compound puts high temperature cabonization in a nitrogen atmosphere, and further roasts in air
Except carbon elimination is to get poriferous titanium dioxide ball.
Further, in step 1), the titanium dioxide precursor is the hydrolysate of butyl titanate.That is, fresh system
Standby titanium dioxide nano-particle is dissolved in dilute hydrochloric acid, obtains four chlorinations of the Low acid that concentration of hydrochloric acid is 0.1-2.0mol/L
Titanium solution.
Further, in step 1), the titanium dioxide precursor and the mass ratio of m-aminophenyl fluosite ball are
1:0.5-2.0.
Further, in step 2), the temperature of heat treatment is 40-200 degree, and the processing time is 2-24 hours.
Further, roasting of the carburizing temperature at 600-800 degree 2-4 hours, in air in step 3), under nitrogen atmosphere
Temperature is 2-4 hours under 500-600 degree.
Above-mentioned preparation method comprises the following specific steps that:
1) it first by m-aminophenol and formaldehyde according to equimolar ratio, is added in the ammonia spirit that pH is 9-11, stirring 24
After hour, filtering obtains m-aminophenyl fluosite ball, is then distributed to a certain amount of m-aminophenyl fluosite ball
In deionized water, the dilute acid soln of titanium dioxide precursor is added, the titanium dioxide precursor being added and m-aminophenol first
It is in mass ratio 1:0.5-2.0 between urea formaldehyde ball, after stirring 10-24 hours, centrifuge separation obtains m-aminophenol formaldehyde tree
Rouge ball/titanium dioxide precursor compound；
2) then m-aminophenyl fluosite ball/titanium dioxide precursor compound is put into the baking oven of 40-200 degree
Heating is taken out after 2-24 hours；
3) again gained compound is continued to be put into Muffle furnace, is first warming up under 600-800 degree in a nitrogen atmosphere and keeps 2
Then hour carbonization roasts 2 hours except carbon elimination is to get poriferous titanium dioxide ball in air atmosphere under 550 degree.
The present invention compared with the existing technology, by the way that titanium dioxide precursor is added to freshly prepd amino-phenol formaldehyde tree
It in the aqueous dispersions of rouge ball, is filtered after stirring a few hours, is then put into baking oven and stands a period of time, then place it in nitrogen gas
High temperature cabonization under atmosphere, and further roast in air, so that poriferous titanium dioxide ball be made, the preparation method is simply mild,
The size of titanium dioxide pore volume can be adjusted by changing the concentration of titanium dioxide precursor, and low in cost, the period compared with
Short, yield is higher, is worthy of popularization.
[Detailed description of the invention]
Fig. 1 is the scanning electron microscope (SEM) photograph of obtained TiO 2 porous ball in the embodiment of the present invention 1.
[specific embodiment]
The present invention provides a kind of method for preparing poriferous titanium dioxide ball, include the following steps: body before titanium dioxide
Body is added in m-aminophenyl fluosite ball dispersion liquid, and stirring a period of time then obtains m-aminophenyl after centrifuge separation
Fluosite ball/titanium dioxide precursor compound；It is again that m-aminophenyl fluosite ball/titanium dioxide precursor is compound
Object is put into placement in the baking oven of certain temperature and is heat-treated for a period of time；By the m-aminophenol formaldehyde tree through Overheating Treatment
Rouge ball/titanium dioxide precursor compound high temperature cabonization in a nitrogen atmosphere, then in air roasting except carbon elimination is to get porous
Titanium dioxide ball.
The type of titanium dioxide precursor used is the hydrolysate of butyl titanate, i.e., freshly prepared titanium dioxide
Nanoparticle is dissolved in dilute hydrochloric acid, obtains the titanium tetrachloride solution of Low acid (concentration of hydrochloric acid 0.1-2.0mol/L).Dioxy
The mass ratio for changing titanium precursor and m-aminophenyl fluosite is 1:0.5-2.0.The temperature of heat treatment is in 40-200 degree, processing
Time is 2-24 hours.Maturing temperature 500-600 of the carburizing temperature at 600-800 degree 2-4 hours, in air under nitrogen atmosphere
Degree is 2-4 hours lower.
The specific steps of above-mentioned preparation method are as follows: first by m-aminophenol and formaldehyde according to equimolar ratio, being added to pH is
In the ammonia spirit of 9-11, after stirring 24 hours, filtering obtains spherical m-aminophenyl fluosite.It then will be a certain amount of
Resin balls are distributed in deionized water, and the dilute acid soln of the precursor of titanium dioxide is added, the titanium dioxide precursor being added
It is in mass ratio 1:0.5-2.0 between m-aminophenyl fluosite ball, after stirring 10-24 hours, centrifuge separation obtains height
Molecule resin balls/titanium dioxide precursor composition compound.Then by macromolecule resin ball/titanium dioxide precursor composition
Compound is put into heated 2-24 hours in the baking oven of 40-200 degree after take out, compound is continued to be put into Muffle furnace, first in nitrogen
It keeps being carbonized for 2 hours under temperature programming to 600-800 degree under gas atmosphere, then roasts 2 hours and remove under 550 degree in air atmosphere
Carbon elimination to get arrive porous spherical titanium dioxide.
The present invention is made combined with specific embodiments below further explained below:
Embodiment 1
(1) preparation of m-aminophenyl fluosite ball: toward 30 containing 24 grams of deionized waters and 10 milliliters of dehydrated alcohols
It spends in solution and 2.0 gram 25% of ammonium hydroxide is added, be added 0.71 gram of m-aminophenol, after stirring and dissolving, 35% formaldehyde is then added
1.0 grams of solution, continue stirring 24 hours, centrifuge separation is 12 hours dry in 50 degree of baking oven by sample.
(2) preparation of titanium dioxide precursor solution: taking 1 milliliter of butyl titanate to be distributed in deionized water, stirring 30
Centrifugal filtration after minute, is washed three times with dehydrated alcohol, 2 hours dry in 50 degree of baking ovens, takes 1 gram of sample 0.1-
2.0mol.L-115 milliliters of hydrochloric acid dissolution, obtain the titanium tetrachloride solution of Low acid.
(3) 0.5 gram of m-aminophenyl fluosite ball is distributed in 20 milliliters of water, 15 milliliters of 0.1mol.L is added-1's
Titanium tetrachloride solution (containing 1 milliliter of butyl titanate), stirring is taken out after 24 hours, is put into 40 degree of baking oven, and it is small to stand 24
Shi Hou takes out, and is put into tube furnace 600 degree of carbonizations under nitrogen atmosphere, and after cooling, it is small to continue 500 degree of lower roastings 2 in air
When, obtain TiO 2 porous ball.
It is as shown in Fig. 1 the scanning electron microscope (SEM) photograph of spherical titanium dioxide porous material, sample particle is probably in 680-940nm
Between.
Embodiment 2
(1) preparation of m-aminophenyl fluosite ball: toward 30 containing 24 grams of deionized waters and 10 milliliters of dehydrated alcohols
It spends in solution and 2.0 gram 25% of ammonium hydroxide is added, be added 0.71 gram of m-aminophenol, after stirring and dissolving, 35% formaldehyde is then added
1.0 grams of solution, continue stirring 24 hours, centrifuge separation is 12 hours dry in 50 degree of baking oven by sample.
(2) preparation of titanium dioxide precursor solution: taking 1 milliliter of butyl titanate to be distributed in deionized water, stirring 30
Centrifugal filtration after minute, is washed three times with dehydrated alcohol, 24 hours dry in 100 degree of baking ovens, takes 1 gram of sample 1.0mol.L-1
15 milliliters of hydrochloric acid dissolution, obtain the titanium tetrachloride solution of Low acid.
(3) 1.0 grams of m-aminophenyl fluosite balls are distributed in 20 milliliters of water, 15 milliliters of 0.5mol.L is added-1's
Titanium tetrachloride solution (containing 1 milliliter of butyl titanate), stirring is taken out after 24 hours, is put into 100 degree of baking oven, and it is small to stand 12
Shi Hou takes out, and is put into tube furnace 800 degree of carbonizations under nitrogen atmosphere, and after cooling, it is small to continue 600 degree of lower roastings 2 in air
When, obtain TiO 2 porous ball.
Embodiment 3
(1) preparation of m-aminophenyl fluosite ball: toward 30 containing 24 grams of deionized waters and 10 milliliters of dehydrated alcohols
It spends in solution and 2.0 gram 25% of ammonium hydroxide is added, be added 0.71 gram of m-aminophenol, after stirring and dissolving, 35% formaldehyde is then added
1.0 grams of solution, continue stirring 24 hours, centrifuge separation.Sample is 12 hours dry in 50 degree of baking oven.
(2) preparation of titanium dioxide precursor solution: taking 1 milliliter of butyl titanate to be distributed in deionized water, stirring 30
Centrifugal filtration after minute, is washed three times with dehydrated alcohol, 2 hours dry in 50 degree of baking ovens, takes 1 gram of sample 0.1-
2.0mol.L-115 milliliters of hydrochloric acid dissolution, obtain the titanium tetrachloride solution of Low acid.
(3) 1.5 grams of m-aminophenyl fluosite balls are distributed in 20 milliliters of water, 15 milliliters of 1.0mol.L is added-1's
Titanium tetrachloride solution (containing 1 milliliter of butyl titanate), stirring is taken out after 24 hours, is put into the baking oven of 40-200 degree, stands 2
It after hour, takes out, is put into tube furnace 750 degree of carbonizations under nitrogen atmosphere, after cooling, it is small to continue 550 degree of lower roastings 2 in air
When, obtain TiO 2 porous ball.
Embodiment 4
(1) preparation of m-aminophenyl fluosite ball: toward 30 containing 24 grams of deionized waters and 10 milliliters of dehydrated alcohols
It spends in solution and 2.0 gram 25% of ammonium hydroxide is added, be added 0.71 gram of m-aminophenol, after stirring and dissolving, 35% formaldehyde is then added
1.0 grams of solution, continue stirring 24 hours, centrifuge separation is 12 hours dry in 50 degree of baking oven by sample.
(2) preparation of titanium dioxide precursor solution: taking 1 milliliter of butyl titanate to be distributed in deionized water, stirring 30
Centrifugal filtration after minute, is washed three times with dehydrated alcohol, 2 hours dry in 50 degree of baking ovens, takes 1 gram of sample 0.1-
2.0mol.L-115 milliliters of hydrochloric acid dissolution, obtain the titanium tetrachloride solution of Low acid.
(3) 2.0 grams of m-aminophenyl fluosite balls are distributed in 20 milliliters of water, 15 milliliters of 2.0mol.L is added-1's
Titanium tetrachloride solution (containing 1 milliliter of butyl titanate), stirring is taken out after 24 hours, is put into 150 degree of baking oven, and it is small to stand 10
Shi Hou takes out, and is put into tube furnace 800 degree of carbonizations under nitrogen atmosphere, and after cooling, it is small to continue 550 degree of lower roastings 2 in air
When, obtain TiO 2 porous ball.
The present invention is simultaneously not limited to the embodiments described above, other any without departing from spiritual essence and principle of the invention
Changes, modifications, substitutions, combinations, simplifications made by lower, should be equivalent substitute mode, are included in protection model of the invention
Within enclosing.
Claims (7)
1. a kind of method for preparing poriferous titanium dioxide ball, which comprises the following steps:
1) titanium dioxide precursor is added in the dispersion liquid of m-aminophenyl fluosite ball, stirs centrifugation point after a few hours
From obtaining m-aminophenyl fluosite ball/titanium dioxide precursor compound；
2) it by the resulting m-aminophenyl fluosite ball/titanium dioxide precursor compound of step 1), is put into baking oven and stands
A period of time is heat-treated；
3) m-aminophenyl fluosite ball/titanium dioxide precursor compound through Overheating Treatment is put high in a nitrogen atmosphere
Temperature carbonization, and further roasting removes carbon elimination to get poriferous titanium dioxide ball in air.
2. the method as described in claim 1, it is characterised in that: in step 1), the titanium dioxide precursor is four fourth of metatitanic acid
Ester hydrolysis product.
3. method according to claim 2, it is characterised in that: the hydrolysate of the butyl titanate is, freshly prepared
Titanium dioxide nano-particle is dissolved in dilute hydrochloric acid, and the titanium tetrachloride for obtaining the Low acid that concentration of hydrochloric acid is 0.1-2.0mol/L is molten
Liquid.
4. the method as described in claim 1, it is characterised in that: in step 1), the titanium dioxide precursor and m-aminophenyl
The mass ratio of fluosite ball is 1:0.5-2.0.
5. the method as described in claim 1, it is characterised in that: in step 2), the temperature of heat treatment is 40-200 degree, when processing
Between be 2-24 hours.
6. the method as described in claim 1, it is characterised in that: in step 3), the carburizing temperature under nitrogen atmosphere is in 600-800
Degree 2-4 hours, the maturing temperature in air is 2-4 hours under 500-600 degree.
7. the method as described in claim 1, which is characterized in that comprise the following specific steps that:
1) it first by m-aminophenol and formaldehyde according to equimolar ratio, is added in the ammonia spirit that pH is 9-11, stirs 24 hours
Afterwards, filter, obtain m-aminophenyl fluosite ball, then by a certain amount of m-aminophenyl fluosite ball be distributed to from
In sub- water, the dilute acid soln of titanium dioxide precursor is added, the titanium dioxide precursor being added and m-aminophenol formaldehyde tree
It is in mass ratio 1:0.5-2.0 between rouge ball, after stirring 10-24 hours, centrifuge separation obtains m-aminophenyl fluosite
Ball/titanium dioxide precursor compound；
2) then m-aminophenyl fluosite ball/titanium dioxide precursor compound is put into the baking oven of 40-200 degree and is heated
It is taken out after 2-24 hours；
3) again gained compound is continued to be put into Muffle furnace, is first warming up under 600-800 degree and is kept for 2 hours in a nitrogen atmosphere
Then carbonization roasts 2 hours except carbon elimination is to get poriferous titanium dioxide ball in air atmosphere under 550 degree.
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| CN201811545342.6A CN109626423A (en) | 2018-12-17 | 2018-12-17 | A method of preparing poriferous titanium dioxide ball |
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| CN201811545342.6A CN109626423A (en) | 2018-12-17 | 2018-12-17 | A method of preparing poriferous titanium dioxide ball |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110416520A (en) * | 2019-07-31 | 2019-11-05 | 安徽相源新能源有限公司 | A kind of preparation process of high discharge capacity stable type lithium cell |
| CN110993367A (en) * | 2019-12-18 | 2020-04-10 | 上海应用技术大学 | Spherical carbon @ manganese oxide @ carbon @ iron oxide composite material and preparation and application thereof |
| CN114551891A (en) * | 2022-04-27 | 2022-05-27 | 潍坊科技学院 | Tin disulfide/titanium dioxide/carbon composite material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386742A (en) * | 2014-11-14 | 2015-03-04 | 上海应用技术学院 | Mesoporous titanium dioxide having high crystallinity and large specific surface area and preparation method thereof |
-
2018
- 2018-12-17 CN CN201811545342.6A patent/CN109626423A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386742A (en) * | 2014-11-14 | 2015-03-04 | 上海应用技术学院 | Mesoporous titanium dioxide having high crystallinity and large specific surface area and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110416520A (en) * | 2019-07-31 | 2019-11-05 | 安徽相源新能源有限公司 | A kind of preparation process of high discharge capacity stable type lithium cell |
| CN110416520B (en) * | 2019-07-31 | 2020-11-06 | 安徽相源新能源有限公司 | Preparation process of high-discharge-capacity stable lithium battery cell |
| CN110993367A (en) * | 2019-12-18 | 2020-04-10 | 上海应用技术大学 | Spherical carbon @ manganese oxide @ carbon @ iron oxide composite material and preparation and application thereof |
| CN114551891A (en) * | 2022-04-27 | 2022-05-27 | 潍坊科技学院 | Tin disulfide/titanium dioxide/carbon composite material and preparation method and application thereof |
| CN114551891B (en) * | 2022-04-27 | 2022-06-24 | 潍坊科技学院 | Tin disulfide/titanium dioxide/carbon composite material and preparation method and application thereof |
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