CN108751252B - Preparation method of titanium dioxide with controllable particle size - Google Patents
Preparation method of titanium dioxide with controllable particle size Download PDFInfo
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Abstract
The invention discloses a preparation method of titanium dioxide with controllable particle size, which comprises the following steps: step 1, adding ethyl cellulose into absolute ethyl alcohol, and stirring until the ethyl cellulose is completely dissolved to obtain a dispersed alcohol solution; step 2, slowly dripping n-butyl titanate into the dispersed alcohol solution, uniformly stirring, and standing at a low temperature to obtain a titanium alcohol solution; step 3, adding methyl cellulose into the titanium alcohol solution, and performing ultrasonic dispersion to form a precipitation solution; step 4, slowly dripping distilled water into the precipitation solution, uniformly stirring at a low temperature until the dripping is finished, then carrying out low-temperature ultrasonic reaction for 2-4h, heating the ultrasonic reaction for 2-4h, and keeping the temperature constant to obtain a suspension sol solution; step 5, filtering the suspension sol solution, and washing with absolute ethyl alcohol at constant temperature to obtain gel; and 6, adding the gel into an ultrasonic reaction kettle, performing circulating water bath ultrasonic reaction for 2-5 hours, cooling and filtering to obtain the nano titanium dioxide. The invention adopts ethyl cellulose as a wrapping agent to wrap the n-butyl titanate, thereby achieving the purpose of indirectly controlling the particle size of the nano titanium dioxide.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of titanium dioxide with controllable particle size.
Background
TiO currently used as one of semiconductor photocatalysts2The photocatalytic material is a novel environment-friendly material which is most researched at present, and the property of the photocatalyst is a key factor in the photocatalytic oxidation process. TiO 22The crystal form, the grain size, the grain diameter, the surface state and other factors have great influence on the photocatalytic performance. The nano-particle with large surface area has good catalytic activity and selectivity due to the surface effect and the volume effect. Nano TiO 22The conduction band energy level and the valence band energy level of the quantum size effect become discrete energy levels due to the quantum size effect, the energy gap is widened, the conduction band potential becomes more negative, and the valence band potential becomes more positive, which means that the quantum size effect has stronger oxidation and reduction capabilities; and because the particle size of the nano particles is small, a photon-generated carrier is easier to migrate to the surface from the inside of the particles than coarse particles, the recombination probability of electrons and holes is obviously reduced, and the photocatalysis performance is also improved. Thus, TiO having a large specific surface area and a small particle diameter is produced2Has been the focus of research in the field of photocatalysis.
With the improvement of living standard of people, environmental materials are paid more attention to by people, and the titanium dioxide photocatalyst has excellent performances of high oxidation activity, strong catalytic performance, stable activity, good moisture resistance, strong sterilization capability and the like, and is widely applied to the aspects of wastewater degradation, harmful gas elimination, sterilization, air purification and the like. However, the existing methods for preparing titanium dioxide powder, such as the traditional solid phase reaction and sintering method, the modern chemical vapor deposition method, the physical vapor deposition method, the chemical vapor infiltration method, the sol-gel method and the like, have the disadvantages of complicated steps, unstable yield, wide particle size distribution range of the prepared particles and difficulty in meeting the requirements of customers.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of titanium dioxide with controllable particle size, which solves the problem of difficult control of the particle size of the existing nano titanium dioxide, and adopts ethyl cellulose as a wrapping agent to wrap n-butyl titanate so as to achieve the aim of indirectly controlling the particle size of the nano titanium dioxide.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of titanium dioxide with controllable particle size comprises the following steps:
step 1, adding ethyl cellulose into absolute ethyl alcohol, and stirring until the ethyl cellulose is completely dissolved to obtain a dispersed alcohol solution;
step 2, slowly dripping n-butyl titanate into the dispersed alcohol solution, uniformly stirring, and standing at a low temperature to obtain a titanium alcohol solution;
step 3, adding methyl cellulose into the titanium alcohol solution, and performing ultrasonic dispersion to form a precipitation solution;
step 4, slowly dripping distilled water into the precipitation solution, uniformly stirring at a low temperature until the dripping is finished, then carrying out low-temperature ultrasonic reaction for 2-4h, heating the ultrasonic reaction for 2-4h, and keeping the temperature constant to obtain a suspension sol solution;
step 5, filtering the suspension sol solution, and washing with absolute ethyl alcohol at constant temperature to obtain gel;
and 6, adding the gel into an ultrasonic reaction kettle, performing circulating water bath ultrasonic reaction for 2-5 hours, cooling and filtering to obtain the nano titanium dioxide.
The concentration of the ethyl cellulose in the absolute ethyl alcohol in the step 1 is 50-100g/L, and the stirring speed of the stirring is 800-1400 r/min.
The adding amount of the n-butyl titanate in the step 2 is 130-170% of the mass of the ethyl cellulose, the stirring speed of the stirring is 500-800r/min, the temperature of the low-temperature standing is 1-7 ℃, and the standing time is 1-3 h.
The adding amount of the methyl cellulose in the step 3 is 60-80% of the mass of the ethyl cellulose.
The temperature of ultrasonic dispersion in the step 3 is 50-60 ℃, and the ultrasonic frequency is 20-25 kHz.
The adding amount of the distilled water in the step 4 is 90-130% of the mass of the absolute ethyl alcohol, the slowly dropwise adding speed is 1-3mL/min, the low-temperature stirring temperature is 0-5 ℃, and the stirring speed is 1000-2000 r/min.
The temperature of the low-temperature ultrasonic reaction in the step 4 is 5-10 ℃, the ultrasonic frequency is 20-30kHz, the temperature of the heating ultrasonic reaction is 60-70 ℃, the ultrasonic frequency is 50-80kHz, and the constant temperature is 70-75 ℃.
The temperature for washing the absolute ethyl alcohol in the step 5 at constant temperature is 60-70 ℃.
And (3) adding absolute ethyl alcohol again after the washing of the ethyl alcohol in the step (5) is finished, and then stirring and distilling to obtain gel, wherein the stirring and distilling temperature is 75-85 ℃, and the stirring speed is 1000-2000 r/min.
The ultrasonic frequency of the circulating water bath ultrasonic reaction in the step 6 is 50-70kHz, the temperature range of the circulating water bath is 20-50 ℃, and the circulation period is 10-20 min.
Step 1, dissolving ethyl cellulose in absolute ethyl alcohol, and forming quick dissolution under the stirring condition to obtain a dispersed alcohol solution.
Step 2, dissolving n-butyl titanate in the dispersing alcohol solution, so that the n-butyl titanate can be uniformly dispersed in the ethanol solution; ethyl cellulose is used as a dispersant to disperse n-butyl titanate and is also used as a wrapping agent to wrap the n-butyl titanate material to form a wrapping and dispersing state.
And 3, adding the methyl cellulose into the titanium alcohol solution to form suspended particles, depositing the suspended particles at the bottom of the ethanol, opening a gap in the wrapped n-butyl titanate under the ultrasonic condition, and allowing the dissipated ethyl cellulose to act on the surface of the methyl cellulose to form a dispersion system, wherein the methyl cellulose is in a suspended state and uniformly distributed in the absolute ethanol.
Step 4, adding distilled water into the precipitation solution, and performing contact reaction on the exposed surface of the n-butyl titanate and the distilled water to achieve a hydrolysis effect; the titanium dioxide is hydrolyzed to form nano titanium dioxide, the suspension dispersion effect is achieved under the action of ethyl cellulose, and meanwhile, the methyl cellulose can be dissolved by the distilled water and acts on the surface of the nano titanium dioxide to form a suspension liquid state; the low-temperature ultrasonic reaction process can ensure that the nano titanium dioxide is dispersed in a distilled water and ethanol system, and the low-temperature condition can ensure that the methyl cellulose is dissolved in water, does not form sol and keeps a dissolved state; in the process of heating and ultrasonic treatment, the methyl cellulose slowly forms sol along with the rise of temperature, the sol is gradually converted into gel, the nano titanium dioxide is solidified in the gel, the gel is continuously broken and solidified along with the action of ultrasonic treatment, and the gel liquid is obtained under the condition of constant temperature after the reaction is finished.
And 5, filtering the anhydrous ethanol containing the ethyl cellulose in a filtering mode to obtain gel coated with the titanium dioxide nano particles, washing the residual ethyl cellulose under constant-temperature washing of the anhydrous ethanol, and keeping the methyl cellulose to be gelatinized under constant-temperature conditions.
Step 6, methyl cellulose can be continuously converted in gel and dissolution through circulating water bath ultrasonic reaction, and the ultrasonic clutch energy can form passivation under the exposure of the nano titanium dioxide to prevent agglomeration, and meanwhile, the ultrasonic clutch energy has enough energy to convert the nano titanium dioxide into an anatase type; dissolving methyl cellulose in water under the cooling condition to form a nano titanium dioxide suspension, and filtering to obtain the nano titanium dioxide.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of difficult control of the particle size of the existing nano titanium dioxide, adopts ethyl cellulose as a wrapping agent to wrap n-butyl titanate, and achieves the aim of indirectly controlling the particle size of the nano titanium dioxide.
2. The invention ensures the dispersion effect in the hydrolysis process of the nano titanium dioxide through the dispersibility of the methyl cellulose and the ethyl cellulose, and can ensure the wrapping effect on the surface of the nano titanium dioxide.
3. The invention fully utilizes the solubility change of different dispersants in different solvents to achieve the effect of stable conversion and obtain double control of formed particle size.
4. The waste liquid obtained by the invention contains a large amount of dispersant, and can be recycled and fully utilized.
Detailed Description
A specific embodiment of the present invention will be described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of titanium dioxide with controllable particle size comprises the following steps:
step 1, adding ethyl cellulose into absolute ethyl alcohol, and stirring until the ethyl cellulose is completely dissolved to obtain a dispersed alcohol solution;
step 2, slowly dripping n-butyl titanate into the dispersed alcohol solution, uniformly stirring, and standing at a low temperature to obtain a titanium alcohol solution;
step 3, adding methyl cellulose into the titanium alcohol solution, and performing ultrasonic dispersion to form a precipitation solution;
step 4, slowly dripping distilled water into the precipitation solution, uniformly stirring at a low temperature until the dripping is finished, then carrying out low-temperature ultrasonic reaction for 2 hours, heating the ultrasonic reaction for 2 hours, and keeping the temperature constant to obtain a suspension sol solution;
step 5, filtering the suspension sol solution, and washing with absolute ethyl alcohol at constant temperature to obtain gel;
and 6, adding the gel into an ultrasonic reaction kettle, performing circulating water bath ultrasonic reaction for 2 hours, cooling and filtering to obtain the nano titanium dioxide.
The concentration of the ethyl cellulose in the step 1 in the absolute ethyl alcohol is 50g/L, and the stirring speed of the stirring is 800 r/min.
The adding amount of the n-butyl titanate in the step 2 is 130% of the mass of the ethyl cellulose, the stirring speed of the stirring is 500r/min, the temperature of the low-temperature standing is 1 ℃, and the standing time is 1 h.
The addition amount of the methyl cellulose in the step 3 is 60 percent of the mass of the ethyl cellulose.
The temperature of ultrasonic dispersion in the step 3 is 50 ℃, and the ultrasonic frequency is 20 kHz.
The adding amount of the distilled water in the step 4 is 90% of the mass of the absolute ethyl alcohol, the slowly dropwise adding speed is 1mL/min, the low-temperature stirring temperature is 0 ℃, and the stirring speed is 1000 r/min.
The temperature of the low-temperature ultrasonic reaction in the step 4 is 5 ℃, the ultrasonic frequency is 20kHz, the temperature of the heating ultrasonic reaction is 60 ℃, the ultrasonic frequency is 50kHz, and the constant temperature is 70 ℃.
The temperature for washing the absolute ethyl alcohol at the constant temperature in the step 5 is 60 ℃.
And (3) adding absolute ethyl alcohol again after the washing of the ethyl alcohol in the step (5) is finished, and then stirring and distilling to obtain gel, wherein the stirring and distilling temperature is 75 ℃, and the stirring speed is 1000 r/min.
The ultrasonic frequency of the circulating water bath ultrasonic reaction in the step 6 is 50kHz, the temperature range of the circulating water bath is 20-50 ℃, and the circulation period is 10 min.
Example 2
A preparation method of titanium dioxide with controllable particle size comprises the following steps:
step 1, adding ethyl cellulose into absolute ethyl alcohol, and stirring until the ethyl cellulose is completely dissolved to obtain a dispersed alcohol solution;
step 2, slowly dripping n-butyl titanate into the dispersed alcohol solution, uniformly stirring, and standing at a low temperature to obtain a titanium alcohol solution;
step 3, adding methyl cellulose into the titanium alcohol solution, and performing ultrasonic dispersion to form a precipitation solution;
step 4, slowly dripping distilled water into the precipitation solution, uniformly stirring at a low temperature until the dripping is finished, then carrying out low-temperature ultrasonic reaction for 4 hours, heating the ultrasonic reaction for 4 hours, and keeping the temperature constant to obtain a suspension sol solution;
step 5, filtering the suspension sol solution, and washing with absolute ethyl alcohol at constant temperature to obtain gel;
and 6, adding the gel into an ultrasonic reaction kettle, performing circulating water bath ultrasonic reaction for 5 hours, cooling and filtering to obtain the nano titanium dioxide.
The concentration of the ethyl cellulose in the step 1 in the absolute ethyl alcohol is 100g/L, and the stirring speed of the stirring is 1400 r/min.
The adding amount of the n-butyl titanate in the step 2 is 170% of the mass of the ethyl cellulose, the stirring speed of the stirring is 800r/min, the low-temperature standing temperature is 7 ℃, and the standing time is 3 hours.
The addition amount of the methyl cellulose in the step 3 is 80 percent of the mass of the ethyl cellulose.
The temperature of ultrasonic dispersion in the step 3 is 60 ℃, and the ultrasonic frequency is 25 kHz.
The adding amount of the distilled water in the step 4 is 130% of the mass of the absolute ethyl alcohol, the slowly dropwise adding speed is 3mL/min, the low-temperature stirring temperature is 5 ℃, and the stirring speed is 2000 r/min.
The temperature of the low-temperature ultrasonic reaction in the step 4 is 10 ℃, the ultrasonic frequency is 30kHz, the temperature of the heating ultrasonic reaction is 70 ℃, the ultrasonic frequency is 80kHz, and the constant temperature is 75 ℃.
The temperature for washing the absolute ethyl alcohol in the step 5 at the constant temperature is 70 ℃.
And (3) adding absolute ethyl alcohol again after the washing of the ethyl alcohol in the step (5) is finished, and then stirring and distilling to obtain gel, wherein the temperature of the stirring and distilling is 85 ℃, and the stirring speed is 2000 r/min.
The ultrasonic frequency of the circulating water bath ultrasonic reaction in the step 6 is 70kHz, the temperature range of the circulating water bath is 20-50 ℃, and the circulation period is 20 min.
Example 3
A preparation method of titanium dioxide with controllable particle size comprises the following steps:
step 1, adding ethyl cellulose into absolute ethyl alcohol, and stirring until the ethyl cellulose is completely dissolved to obtain a dispersed alcohol solution;
step 2, slowly dripping n-butyl titanate into the dispersed alcohol solution, uniformly stirring, and standing at a low temperature to obtain a titanium alcohol solution;
step 3, adding methyl cellulose into the titanium alcohol solution, and performing ultrasonic dispersion to form a precipitation solution;
step 4, slowly dripping distilled water into the precipitation solution, uniformly stirring at a low temperature until the dripping is finished, then carrying out low-temperature ultrasonic reaction for 3 hours, heating the ultrasonic reaction for 3 hours, and keeping the temperature constant to obtain a suspension sol solution;
step 5, filtering the suspension sol solution, and washing with absolute ethyl alcohol at constant temperature to obtain gel;
and 6, adding the gel into an ultrasonic reaction kettle, performing circulating water bath ultrasonic reaction for 4 hours, cooling and filtering to obtain the nano titanium dioxide.
The concentration of the ethyl cellulose in the absolute ethyl alcohol in the step 1 is 80g/L, and the stirring speed of the stirring is 1200 r/min.
The adding amount of the n-butyl titanate in the step 2 is 150% of the mass of the ethyl cellulose, the stirring speed of the stirring is 600r/min, the temperature of the low-temperature standing is 4 ℃, and the standing time is 2 hours.
The addition amount of the methyl cellulose in the step 3 is 70 percent of the mass of the ethyl cellulose.
The temperature of ultrasonic dispersion in the step 3 is 55 ℃, and the ultrasonic frequency is 23 kHz.
The adding amount of the distilled water in the step 4 is 120% of the mass of the absolute ethyl alcohol, the slowly dropwise adding speed is 2mL/min, the low-temperature stirring temperature is 2 ℃, and the stirring speed is 1500 r/min.
The temperature of the low-temperature ultrasonic reaction in the step 4 is 8 ℃, the ultrasonic frequency is 25kHz, the temperature of the heating ultrasonic reaction is 65 ℃, the ultrasonic frequency is 70kHz, and the constant temperature is 73 ℃.
The temperature for washing the absolute ethyl alcohol in the step 5 at the constant temperature is 65 ℃.
And (3) adding absolute ethyl alcohol again after the washing of the ethyl alcohol in the step (5) is finished, and then stirring and distilling to obtain gel, wherein the stirring and distilling temperature is 80 ℃, and the stirring speed is 1500 r/min.
The ultrasonic frequency of the circulating water bath ultrasonic reaction in the step 6 is 60kHz, the temperature range of the circulating water bath is 20-50 ℃, and the circulation period is 15 min.
Performance detection
In summary, the invention has the following advantages:
1. the invention solves the problem of difficult control of the particle size of the existing nano titanium dioxide, adopts ethyl cellulose as a wrapping agent to wrap n-butyl titanate, and achieves the aim of indirectly controlling the particle size of the nano titanium dioxide.
2. The invention ensures the dispersion effect in the hydrolysis process of the nano titanium dioxide through the dispersibility of the methyl cellulose and the ethyl cellulose, and can ensure the wrapping effect on the surface of the nano titanium dioxide.
3. The invention fully utilizes the solubility change of different dispersants in different solvents to achieve the effect of stable conversion and obtain double control of formed particle size.
4. The waste liquid obtained by the invention contains a large amount of dispersant, and can be recycled and fully utilized.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. A preparation method of titanium dioxide with controllable particle size is characterized in that: the method comprises the following steps:
step 1, adding ethyl cellulose into absolute ethyl alcohol, and stirring until the ethyl cellulose is completely dissolved to obtain a dispersed alcohol solution;
step 2, slowly dripping n-butyl titanate into the dispersed alcohol solution, uniformly stirring, and standing at a low temperature to obtain a titanium alcohol solution;
step 3, adding methyl cellulose into the titanium alcohol solution, and performing ultrasonic dispersion to form a precipitation solution;
step 4, slowly dripping distilled water into the precipitation solution, uniformly stirring at a low temperature until the dripping is finished, then carrying out low-temperature ultrasonic reaction for 2-4h, heating the ultrasonic reaction for 2-4h, and keeping the temperature constant to obtain a suspension sol solution;
step 5, filtering the suspension sol solution, and washing with absolute ethyl alcohol at constant temperature to obtain gel;
and 6, adding the gel into an ultrasonic reaction kettle, performing circulating water bath ultrasonic reaction for 2-5 hours, cooling and filtering to obtain the nano titanium dioxide.
2. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the concentration of the ethyl cellulose in the absolute ethyl alcohol in the step 1 is 50-100g/L, and the stirring speed of the stirring is 800-1400 r/min.
3. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the adding amount of the n-butyl titanate in the step 2 is 130-170% of the mass of the ethyl cellulose, the stirring speed of the stirring is 500-800r/min, the temperature of the low-temperature standing is 1-7 ℃, and the standing time is 1-3 h.
4. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the adding amount of the methyl cellulose in the step 3 is 60-80% of the mass of the ethyl cellulose.
5. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the temperature of ultrasonic dispersion in the step 3 is 50-60 ℃, and the ultrasonic frequency is 20-25 kHz.
6. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the adding amount of the distilled water in the step 4 is 90-130% of the mass of the absolute ethyl alcohol, the slowly dropwise adding speed is 1-3mL/min, the low-temperature stirring temperature is 0-5 ℃, and the stirring speed is 1000-2000 r/min.
7. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the temperature of the low-temperature ultrasonic reaction in the step 4 is 5-10 ℃, the ultrasonic frequency is 20-30kHz, the temperature of the heating ultrasonic reaction is 60-70 ℃, the ultrasonic frequency is 50-80kHz, and the constant temperature is 70-75 ℃.
8. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the temperature for washing the absolute ethyl alcohol in the step 5 at constant temperature is 60-70 ℃.
9. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: and (3) adding absolute ethyl alcohol again after the washing of the ethyl alcohol in the step (5) is finished, and then stirring and distilling to obtain gel, wherein the stirring and distilling temperature is 75-85 ℃, and the stirring speed is 1000-2000 r/min.
10. The method for preparing titanium dioxide with controllable particle size according to claim 1, wherein: the ultrasonic frequency of the circulating water bath ultrasonic reaction in the step 6 is 50-70kHz, the temperature range of the circulating water bath is 20-50 ℃, and the circulation period is 10-20 min.
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| CN109205664A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of method that electrostatic spinning prepares nano-titanium dioxide |
| CN111299591A (en) * | 2020-04-15 | 2020-06-19 | 无锡乐普金属科技有限公司 | Preparation method of tungsten-copper alloy plate |
| CN111410756A (en) * | 2020-04-22 | 2020-07-14 | 无锡嘉弘塑料科技有限公司 | Preparation method of weather-resistant polyvinyl chloride granules |
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| CN115490455B (en) * | 2022-10-09 | 2023-08-18 | 临沂海螺新材料科技有限公司 | Low-doping-amount enhanced cement grinding aid and preparation method thereof |
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| CN1097400A (en) * | 1994-04-28 | 1995-01-18 | 雷亚林 | The manufacture method of super fine powder of titanium dioxide |
| CN105936514A (en) * | 2016-06-12 | 2016-09-14 | 长兴中昊化工有限公司 | Making process of rutile type titanium dioxide nano-powder |
| CN106976907A (en) * | 2017-04-27 | 2017-07-25 | 吴亚良 | A kind of nano titanium oxide preparation method of size tunable |
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|---|---|---|---|---|
| CN1097400A (en) * | 1994-04-28 | 1995-01-18 | 雷亚林 | The manufacture method of super fine powder of titanium dioxide |
| CN105936514A (en) * | 2016-06-12 | 2016-09-14 | 长兴中昊化工有限公司 | Making process of rutile type titanium dioxide nano-powder |
| CN106976907A (en) * | 2017-04-27 | 2017-07-25 | 吴亚良 | A kind of nano titanium oxide preparation method of size tunable |
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