CN111377477A - Preparation method of nano titanium dioxide - Google Patents
Preparation method of nano titanium dioxide Download PDFInfo
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- CN111377477A CN111377477A CN202010263057.6A CN202010263057A CN111377477A CN 111377477 A CN111377477 A CN 111377477A CN 202010263057 A CN202010263057 A CN 202010263057A CN 111377477 A CN111377477 A CN 111377477A
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 151
- 235000019441 ethanol Nutrition 0.000 claims abstract description 61
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000005507 spraying Methods 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 26
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 24
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003223 protective agent Substances 0.000 abstract description 4
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 5
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000005348 self-cleaning glass Substances 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
Abstract
The invention discloses a preparation method of nano titanium dioxide, which comprises the following steps: adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form good dispersed alcohol liquid; adding tetrabutyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid; spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, and decompressing and cooling to obtain a pre-coated substrate; placing the pre-coated substrate in a reaction kettle in a low-humidity environment, standing for 40-60min, and circulating internal air for 20-30min to obtain a coated substrate; soaking the coated substrate in hot ethanol for 20-50min, performing constant temperature ultrasonic treatment for 10-20min, taking out the substrate, filtering while the substrate is hot to obtain precipitate, and washing with hot ethanol to obtain nanometer titanium dioxide. The invention solves the problems of complex process and high energy consumption in the prior art, and forms good coating protective agent and isolating agent by utilizing the solubility change of the sodium dodecyl sulfate in the ethanol, thereby realizing lossless conversion.
Description
Technical Field
The invention belongs to the field of nano materials, relates to the field of photocatalysis, and particularly relates to a preparation method of nano titanium dioxide.
Background
The nano titanium dioxide is white loose powder, has strong ultraviolet shielding effect and good dispersibility and weather resistance. Can be used in the fields of cosmetics, functional fiber, plastics, coating, paint, etc., and can be used as ultraviolet screening agent for preventing ultraviolet ray invasion. Can also be used for top-grade automobile finish paint, and has the effect of color variation along with the angle. With the development of technology, the application field of nano titanium dioxide is continuously expanded, and the nano titanium dioxide is widely applied to ultraviolet-resistant materials, textiles, photocatalytic catalysts, self-cleaning glass, sunscreen cream, coatings, printing ink, food packaging materials, paper industry, aerospace industry and lithium batteries. Among the above industries, the lithium battery industry has a relatively high demand for nano titanium dioxide, and the most basic requirement is that the nano titanium dioxide has uniform particle size; the existing titanium dioxide process mainly adopts extensive type, and although a certain amount of nano titanium dioxide can be produced, the control rate of the particle size distribution of the nano titanium dioxide is not strong, so that the requirement is difficult to meet; although some preparation methods in the current laboratory can achieve good uniformity of nanometer particle size, the preparation process is extremely complex and the energy consumption is extremely high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of nano titanium dioxide, which solves the problems of complex process and high energy consumption in the prior art, and forms a good coating protective agent and a good isolating agent by utilizing the solubility change of sodium dodecyl sulfate in ethanol, thereby realizing lossless conversion.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of nano titanium dioxide comprises the following steps:
step 1, adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form a good dispersed alcohol solution; the concentration of the sodium dodecyl sulfate in the absolute ethyl alcohol is 20-50g/L, and the temperature is 60-70 ℃;
step 2, adding n-butyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid; the concentration of the n-butyl titanate in the absolute ethyl alcohol is 20-50g/L, the low-temperature stirring temperature is 5-10 ℃, and the stirring speed is 1000-2000 r/min;
step 3, spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, and decompressing and cooling to obtain a pre-coated substrate; the spraying amount of the dispersed alcohol solution is 5-10mL/cm2The temperature is 50-60 ℃, the quick drying temperature is 90-100 ℃, and the spraying amount of the titanium liquid is 10-20mL/cm2The temperature is 10-20 ℃, and the temperature for rapid heating is 80-90 ℃;
step 4, placing the pre-coated substrate in a reaction kettle in a low-humidity environment for standing for 40-60min, and circulating internal air for 20-30min to obtain a coated substrate, wherein the humidity in the low-humidity environment is 10-20%, the standing temperature is 80-90 ℃, and the air flow rate of the internal air circulation is 10-20 mL/min;
step 5, soaking the coated substrate in hot ethanol for 20-50min, carrying out constant temperature ultrasound for 10-20min, taking out the substrate, filtering while the substrate is hot to obtain a precipitate, and washing with hot ethanol to obtain nano titanium dioxide; the temperature of the hot ethanol is 60-70 ℃, the temperature of constant temperature ultrasonic treatment is 60-70 ℃, the ultrasonic frequency is 40-60kHz, and the temperature of hot filtration is 60-70 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problems of complex process and high energy consumption in the prior art, and forms good coating protective agent and isolating agent by utilizing the solubility change of the sodium dodecyl sulfate in the ethanol, thereby realizing lossless conversion.
2. The invention utilizes the nano titanium dioxide prepared by the in-situ hydrolysis method and simultaneously fully utilizes the insolubility of the nano titanium dioxide to realize rapid impurity removal.
3. The invention effectively reduces the oxidation-reduction reaction, realizes the full recovery of the raw materials, and greatly reduces the use of the raw materials, thereby reducing the cost.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
A preparation method of nano titanium dioxide comprises the following steps:
step 1, adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form a good dispersed alcohol solution; the concentration of the sodium dodecyl sulfate in the absolute ethyl alcohol is 20-50g/L, the temperature is 60-70 ℃, the sodium dodecyl sulfate has solubility in the hot ethyl alcohol, and stable hot dispersion alcohol liquid can be formed;
step 2, adding n-butyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid; the concentration of the n-butyl titanate in the absolute ethyl alcohol is 20-50g/L, the low-temperature stirring temperature is 5-10 ℃, the stirring speed is 1000-2000r/min, and the solubility of the n-butyl titanate in the ethyl alcohol can ensure that the n-butyl titanate is uniformly dispersed in the absolute ethyl alcohol;
step 3, spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, quickly heating, relieving pressure and cooling to obtain a pre-coated substrate; the spraying amount of the dispersed alcohol solution is 5-10mL/cm2The temperature is 50-60 ℃, the quick drying temperature is 90-100 ℃, and the spraying amount of the titanium liquid is 10-20mL/cm2The temperature is 10-20 ℃, and the temperature for rapid heating is 80-90 ℃; spraying the dispersion alcohol solution onto a substrate while the dispersion alcohol solution is hot, forming a sodium dodecyl sulfate liquid film taking ethanol as a film forming agent on the surface, and quickly drying to quickly remove absolute ethanol to form a sodium dodecyl sulfate film on the surface; the titanium liquid forms fog-like liquid drops in a spraying mode, and the fog-like liquid drops form a liquid film on the sodium dodecyl sulfate at the same time under the temperature condition, and the absolute ethyl alcohol at the temperature has only a slightly soluble effect on the sodium dodecyl sulfate and cannot damage the surface film of the sodium dodecyl sulfate; in the process of rapid heating, the absolute ethyl alcohol in the surface film is rapidly dried and converted into ethanol steam, the n-butyl titanate is further dispersed, and the n-butyl titanate still keeps a liquid drop state and is settled on the surface of the lauryl sodium sulfate film to form a surface liquid film;
step 4, placing the pre-coated substrate in a reaction kettle in a low-humidity environment for standing for 40-60min, and circulating internal air for 20-30min to obtain a coated substrate, wherein the humidity in the low-humidity environment is 10-20%, the standing temperature is 80-90 ℃, and the air flow rate of the internal air circulation is 10-20 mL/min; under a low-humidity environment, the pre-plated film forms a good reaction system with water molecules based on the hydrolysis characteristic of n-butyl titanate, n-butyl titanate is converted into titanic acid and converted into nano titanium dioxide under a temperature condition, meanwhile, the water solubility of sodium dodecyl sulfate can ensure that the water molecules are quickly concentrated, the hydrolysis speed of the n-butyl titanate is greatly accelerated, the internal air circulation can accelerate the air circulation speed, the water molecules are ensured to be fully contacted with the n-butyl titanate, and the conversion rate of the n-butyl titanate is greatly improved;
step 5, soaking the coated substrate in hot ethanol for 20-50min, carrying out constant temperature ultrasound for 10-20min, taking out the substrate, filtering while the substrate is hot to obtain a precipitate, and washing with hot ethanol to obtain nano titanium dioxide; the temperature of the hot ethanol is 60-70 ℃, the temperature of constant-temperature ultrasound is 60-70 ℃, the ultrasonic frequency is 40-60kHz, the temperature of hot filtration is 60-70 ℃, the lauryl sodium sulfate can form good solubility under the condition of the hot ethanol, the substrate and the nano titanium dioxide are disconnected to form a nano titanium dioxide dispersion system, and the lauryl sodium sulfate is dissolved in the hot ethanol, can play a role of a surfactant and improve the dispersion effect of the nano titanium dioxide; after hot filtration, the nano titanium dioxide is directly separated out as a precipitate, and the nano titanium dioxide is cleaned by utilizing the pyrolysis property of hot ethanol to lauryl sodium sulfate to obtain pure nano titanium dioxide.
Example 1
A preparation method of nano titanium dioxide comprises the following steps:
step 1, adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form a good dispersed alcohol solution; the concentration of the sodium dodecyl sulfate in the absolute ethyl alcohol is 20g/L, and the temperature is 60 ℃;
step 2, adding n-butyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid; the concentration of the n-butyl titanate in the absolute ethyl alcohol is 20g/L, the low-temperature stirring temperature is 5 ℃, and the stirring speed is 1000 r/min;
step 3, spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, and decompressing and cooling to obtain a pre-coated substrate; the spraying amount of the dispersed alcohol solution is 5mL/cm2The temperature is 50 ℃, the temperature for quick drying is 90 ℃, and the spraying amount of the titanium liquid is 10mL/cm2The temperature is 10 ℃, and the temperature for rapidly raising the temperature is 80 ℃;
step 4, placing the pre-coated substrate in a reaction kettle in a low-humidity environment for standing for 40min, and circulating internal air for 20-30min to obtain a coated substrate, wherein the humidity in the low-humidity environment is 10%, the standing temperature is 80-90 ℃, and the air flow rate of the internal air circulation is 10 mL/min;
step 5, soaking the coated substrate in hot ethanol for 20min, carrying out constant-temperature ultrasound for 10min, taking out the substrate, filtering while the substrate is hot to obtain a precipitate, and washing with hot ethanol to obtain nano titanium dioxide; the temperature of the hot ethanol is 60 ℃, the temperature of constant temperature ultrasonic is 60 ℃, the ultrasonic frequency is 40kHz, and the temperature of hot filtering is 60 ℃.
The particle size of the nano titanium dioxide in the embodiment is 100-200nm, and the distribution rate is 97.3%.
Example 2
A preparation method of nano titanium dioxide comprises the following steps:
step 1, adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form a good dispersed alcohol solution; the concentration of the sodium dodecyl sulfate in the absolute ethyl alcohol is 50g/L, and the temperature is 70 ℃;
step 2, adding n-butyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid; the concentration of the n-butyl titanate in the absolute ethyl alcohol is 50g/L, the low-temperature stirring temperature is 10 ℃, and the stirring speed is 2000 r/min;
step 3, spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, and decompressing and cooling to obtain a pre-coated substrate; the spraying amount of the dispersed alcohol solution is 10mL/cm2The temperature is 60 ℃, the temperature for quick drying is 100 ℃, and the spraying amount of the titanium liquid is 20mL/cm2The temperature is 20 ℃, and the temperature for rapidly raising the temperature is 90 ℃;
step 4, placing the pre-coated substrate in a reaction kettle in a low-humidity environment for standing for 60min, and circulating internal air for 30min to obtain a coated substrate, wherein the humidity in the low-humidity environment is 20%, the standing temperature is 80-90 ℃, and the air flow rate of the internal air circulation is 20 mL/min;
step 5, soaking the coated substrate in hot ethanol for 50min, carrying out constant-temperature ultrasonic treatment for 20min, taking out the substrate, filtering while the substrate is hot to obtain a precipitate, and washing with hot ethanol to obtain nano titanium dioxide; the temperature of the hot ethanol is 70 ℃, the temperature of constant temperature ultrasonic treatment is 70 ℃, the ultrasonic frequency is 60kHz, and the temperature of hot filtration is 70 ℃.
The particle size of the nano titanium dioxide in the embodiment is 300-400nm, and the distribution rate is 98.1%.
Example 3
A preparation method of nano titanium dioxide comprises the following steps:
step 1, adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form a good dispersed alcohol solution; the concentration of the sodium dodecyl sulfate in the absolute ethyl alcohol is 40g/L, and the temperature is 65 ℃;
step 2, adding n-butyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid; the concentration of the n-butyl titanate in the absolute ethyl alcohol is 40g/L, the low-temperature stirring temperature is 8 ℃, and the stirring speed is 1500 r/min;
step 3, spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, and decompressing and cooling to obtain a pre-coated substrate; the spraying amount of the dispersed alcohol solution is 8mL/cm2The temperature is 55 ℃, the temperature for quick drying is 95 ℃, and the spraying amount of the titanium liquid is 15mL/cm2The temperature is 15 ℃, and the temperature for rapidly heating is 85 ℃;
step 4, placing the pre-coated substrate in a reaction kettle in a low-humidity environment for standing for 50min, and circulating internal air for 25min to obtain a coated substrate, wherein the humidity in the low-humidity environment is 15%, the standing temperature is 85 ℃, and the air flow rate of the internal air circulation is 15 mL/min;
step 5, soaking the coated substrate in hot ethanol for 40min, carrying out constant-temperature ultrasound for 15min, taking out the substrate, filtering while the substrate is hot to obtain a precipitate, and washing with hot ethanol to obtain nano titanium dioxide; the temperature of the hot ethanol is 65 ℃, the temperature of constant temperature ultrasonic treatment is 65 ℃, the ultrasonic frequency is 50kHz, and the temperature of hot filtration is 65 ℃.
The particle size of the nano titanium dioxide in the embodiment is 200-300nm, and the distribution rate is 97.7%.
In summary, the invention has the following advantages:
1. the invention solves the problems of complex process and high energy consumption in the prior art, and forms good coating protective agent and isolating agent by utilizing the solubility change of the sodium dodecyl sulfate in the ethanol, thereby realizing lossless conversion.
2. The invention utilizes the nano titanium dioxide prepared by the in-situ hydrolysis method and simultaneously fully utilizes the insolubility of the nano titanium dioxide to realize rapid impurity removal.
3. The invention effectively reduces the oxidation-reduction reaction, realizes the full recovery of the raw materials, and greatly reduces the use of the raw materials, thereby reducing the cost.
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 (6)
1. A preparation method of nano titanium dioxide is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding sodium dodecyl sulfate into absolute ethyl alcohol, heating and stirring uniformly to form a good dispersed alcohol solution;
step 2, adding n-butyl titanate into absolute ethyl alcohol, and uniformly stirring at a low temperature to form uniform titanium liquid;
step 3, spraying the dispersion alcohol solution on a substrate while the dispersion alcohol solution is hot, and quickly drying to obtain a first film layer; then, settling the titanium liquid on the surface of the first film layer by adopting a constant-temperature spraying method, and decompressing and cooling to obtain a pre-coated substrate;
step 4, placing the pre-coated substrate in a reaction kettle in a low-humidity environment for standing for 40-60min, and circulating the internal air for 20-30min to obtain a coated substrate;
and 5, soaking the coated substrate in hot ethanol for 20-50min, carrying out constant-temperature ultrasonic treatment for 10-20min, taking out the substrate, filtering while the substrate is hot to obtain a precipitate, and washing with hot ethanol to obtain the nano titanium dioxide.
2. The method for preparing nano titanium dioxide according to claim 1, characterized in that: the concentration of the sodium dodecyl sulfate in the absolute ethyl alcohol in the step 1 is 20-50g/L, and the temperature is 60-70 ℃.
3. The method for preparing nano titanium dioxide according to claim 1, characterized in that: the concentration of the tetrabutyl titanate in the step 2 in the absolute ethyl alcohol is 20-50g/L, the low-temperature stirring temperature is 5-10 ℃, and the stirring speed is 1000-2000 r/min.
4. The method for preparing nano titanium dioxide according to claim 1, characterized in that: the spraying amount of the dispersing alcohol solution in the step 3 is 5-10mL/cm2The temperature is 50-60 ℃, the quick drying temperature is 90-100 ℃, and the spraying amount of the titanium liquid is 10-20mL/cm2The temperature is 10-20 ℃, and the temperature for rapid temperature rise is 80-90 ℃.
5. The method for preparing nano titanium dioxide according to claim 1, characterized in that: the humidity in the low-humidity environment in the step 4 is 10-20%, the standing temperature is 80-90 ℃, and the air flow rate of the internal air circulation is 10-20 mL/min.
6. The method for preparing nano titanium dioxide according to claim 1, characterized in that: the temperature of the hot ethanol in the step 5 is 60-70 ℃, the temperature of constant temperature ultrasonic treatment is 60-70 ℃, the ultrasonic frequency is 40-60kHz, and the temperature of hot filtering is 60-70 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250101A (en) * | 2020-10-29 | 2021-01-22 | 焦祝根 | Method for in-situ preparation of nano zinc chloride |
| CN112456532A (en) * | 2020-12-08 | 2021-03-09 | 理光感热技术（无锡）有限公司 | Preparation method of calcium carbonate |
-
2020
- 2020-04-07 CN CN202010263057.6A patent/CN111377477A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250101A (en) * | 2020-10-29 | 2021-01-22 | 焦祝根 | Method for in-situ preparation of nano zinc chloride |
| CN112456532A (en) * | 2020-12-08 | 2021-03-09 | 理光感热技术（无锡）有限公司 | Preparation method of calcium carbonate |
| CN112456532B (en) * | 2020-12-08 | 2023-10-24 | 理光感热技术（无锡）有限公司 | Preparation method of calcium carbonate |
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Application publication date: 20200707 |