CN109179498A - A kind of preparation method of hydrophobic type titanium dioxide - Google Patents
A kind of preparation method of hydrophobic type titanium dioxide Download PDFInfo
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- CN109179498A CN109179498A CN201811165089.1A CN201811165089A CN109179498A CN 109179498 A CN109179498 A CN 109179498A CN 201811165089 A CN201811165089 A CN 201811165089A CN 109179498 A CN109179498 A CN 109179498A
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- C—CHEMISTRY; METALLURGY
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- 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
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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
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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Abstract
The invention belongs to technical field of titanium dioxide, and in particular to a kind of preparation method of hydrophobic type titanium dioxide includes the following steps: step 1, tetrabutyl titanate is added and is stirred evenly into dehydrated alcohol, obtains titanium alcohol liquid；Step 2, oleic acid is added to absolute ethanol and is stirred evenly, isothermal reaction 2-4h is then added into pyroreaction kettle, obtain constant temperature atmosphere；Step 3, isothermal reaction 2-5h in the pyroreaction kettle into step 2 is added in titanium alcohol liquid, then microwave reaction 30-150min, gas-solid mixture after constant temperature sedimentation；Step 4, gas slowly is poured in pyroreaction kettle, until mixed gas is discharged, the gas uses nitrogen or inert gas；Step 5, deposit, i.e. hydrophobic nano titanium dioxide will be obtained after pyroreaction kettle cooling pressure release.The present invention solves the problems such as prior art is at high cost, and process is complicated, converts high temperature microwave vapor reaction for the liquid hydrolysis of tetrabutyl titanate, reduces reaction difficulty.
Description
Technical field
The invention belongs to technical field of titanium dioxide, and in particular to a kind of preparation method of hydrophobic type titanium dioxide.
Background technique
In recent years, with the extensive research to wellability, it has been recognized that super-hydrophobic film is in automatically cleaning, miniflow system
And special separation etc. has huge potential application, therefore the preparation of super-hydrophobic film also becomes focus concerned by people.By
Classical Young's equation is it is found that surface can directly determine the wellability on surface, to improve hydrophobicity, it is necessary to reduction table as far as possible
The surface energy of face substance.Although low-surface energy substance can enhance the hydrophobicity of film surface, but still no more than 120 °, another party
Face surface roughness and the hydrophobicity size of film also have close relationship.Therefore, the surface for reducing material can and increase material
The surface roughness of material can improve material surface super-hydrophobicity.Super-hydrophobic film not only has waterproof, dust-proof, anticorrosion, prevents
The functions such as mould also have self-cleaning function, and in waterproof material, building surface and the windshield of automobile etc. have emphatically
The use and wide prospect wanted.
The preparation of usual super hydrophobic surface needs to reduce surface by surface modification fluorocarbons or chain alkyl certainly
Super hydrophobic surface (is prepared with low-surface-energy fluorine material, enrichment of this surface with fluorine-containing group, fluorine-containing groups by energy
Growth, branch chain increase, surface wettability will all reduce, i.e., contact angle increases；Simultaneously because the reduction of surface adhesive, rolling
Dynamic angle is also reducing rapidly).Simultaneously because the contact angle of smooth surface is smaller, therefore also need to construct suitable fine structure
Adjust surface wet.The method of construction rough surface has at present: plasma etching, chemical vapor deposition, electrochemical deposition, gold
Belong to anodic oxidation etc..But the most cost of manufacture of these methods is high, process is complicated, and experiment condition is harsh, it is a wide range of to be difficult to carry out
Manufacture is to limit its application.
Summary of the invention
For the problems of the prior art, the present invention provides a kind of preparation method of hydrophobic type titanium dioxide, solves existing
There is the problems such as process costs are high, and process is complicated, convert high temperature microwave vapor reaction for the liquid hydrolysis of tetrabutyl titanate,
Reduce reaction difficulty.
To realize the above technical purpose, the technical scheme is that
A kind of preparation method of hydrophobic type titanium dioxide, includes the following steps:
Step 1, tetrabutyl titanate is added and is stirred evenly into dehydrated alcohol, obtain titanium alcohol liquid；
Step 2, oleic acid is added to absolute ethanol and is stirred evenly, isothermal reaction 2- is then added into pyroreaction kettle
4h obtains constant temperature atmosphere；
Step 3, isothermal reaction 2-5h in the pyroreaction kettle into step 2 is added in titanium alcohol liquid, then microwave reaction 30-
150min, gas-solid mixture after constant temperature sedimentation；
Step 4, gas slowly is poured in pyroreaction kettle, until mixed gas is discharged, the gas uses nitrogen
Or inert gas；
Step 5, deposit, i.e. hydrophobic nano titanium dioxide will be obtained after pyroreaction kettle cooling pressure release.
Mass concentration of the tetrabutyl titanate in dehydrated alcohol in the step 1 is 50-100g/L, described to stir evenly
Mixing speed be 1000-2000r/min.
Mass concentration of the oleic acid in dehydrated alcohol in the step 2 is 50-100g/L, the mixing speed stirred evenly
For 500-1000r/min.
The pressure of isothermal reaction in the step 2 is 0.3-0.5MPa, and temperature is 350-370 DEG C.
The pressure of isothermal reaction in the step 3 is 0.5-0.7MPa, and temperature is 360-380 DEG C.
The power of microwave reaction in the step 3 is 500-800W, and temperature is 400-420 DEG C, the constant temperature sedimentation
Temperature is 350-360 DEG C.
The speed slowly poured in the step 4 is 50-100mL/min, and temperature is 330-360 DEG C.
Mixed gas in the step 4 can recycle to form oleic acid ethanol after cooling down, in step 2.
The cooling rate of cooling pressure release in the step 5 is 10-20 DEG C/min, and pressure release speed is 0.01-0.02MPa/
min。
Tetrabutyl titanate is dissolved in formation titanium alcohol liquid in dehydrated alcohol by step 1, and tetrabutyl titanate is evenly dispersed to nothing
In water-ethanol.
Oleic acid is dissolved in dehydrated alcohol by step 2, and is formed evenly dispersed, isothermal reaction is then carried out, by oleic acid
Ethanol solution forms gaseous state, and ethyl alcohol and oleic acid are converted into gaseous state at this time, forms high-temperature mixed gas.
Metatitanic acid liquid is added into pyroreaction kettle step 3, and carries out pyroreaction, while being converted into gaseous state, at this time
Tetrabutyl titanate gas, alcohol gas, oleic acid gas are formed in pyroreaction kettle, and it is anti-that microwave is then carried out in pyroreaction kettle
It answers, the valence link of tetrabutyl titanate is broken by the oscillation that microwave generates, and Nano titanium dioxide particle is formed, due to nano-scale particle
Floating dust shape itself is easily formed, and oleic acid surface forms activity-OH, activity-OH and nanometer two since microwave oscillation is by-OH activation
The active group of titania surface forms reaction, achievees the purpose that hydrophobic modification, after constant temperature settlement treatment, modified nanometer
Titanium dioxide constantly deposits, and reaches solid gas separating effect.
Step 4 slowly pours nitrogen or inert gas in pyroreaction kettle, by the mixed gas in pyroreaction kettle
It constantly goes out, guarantees to form nitrogen atmosphere or atmosphere of inert gases in pyroreaction kettle, can not only guarantee oleic acid modified two
The stability of titanium oxide, while also guaranteeing the good separation property of gas-solid.The mixed gas of discharge can be as oleic acid second in step 2
Alcohol mixed gas, achievees the purpose that recycling.
Gas is discharged by way of the pressure release that cools down for step 5, obtains deposit, hydrophobic nano titanium dioxide.
From the above, it can be seen that the present invention has following advantages:
1. the present invention solves the problems such as prior art is at high cost, and process is complicated, the liquid of tetrabutyl titanate is hydrolyzed anti-
It should be converted into high temperature microwave vapor reaction, reduce reaction difficulty.
2. reaction system is converted vapor reaction by the present invention, it is ensured that the dispersibility of nanometer titanium dioxide forming, simultaneously
It is used without dispersing agent, reduces the generation of foreign gas.
3. the nano-titanium dioxide under the effect of hot kinetic energy is formed hydrophobic change with oleic acid gas using microwave reaction by the present invention
Property reaction, improve reaction efficiency, also solve oleic acid and tetrabutyl titanate under the conditions of liquid reacts difficulty.
4. present invention process is simple, exploitativeness is strong, and the exhaust gas mixing that simultaneous reactions generate can reuse, and reduces
The discharge of pollutant, meets national requirements for environmental protection.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to claim of the invention.
Embodiment 1
A kind of preparation method of hydrophobic type titanium dioxide, includes the following steps:
Step 1, tetrabutyl titanate is added and is stirred evenly into dehydrated alcohol, obtain titanium alcohol liquid；
Step 2, oleic acid is added to absolute ethanol and is stirred evenly, isothermal reaction 2h is then added into pyroreaction kettle,
Obtain constant temperature atmosphere；
Step 3, isothermal reaction 2h in the pyroreaction kettle into step 2 is added in titanium alcohol liquid, then microwave reaction
30min, gas-solid mixture after constant temperature sedimentation；
Step 4, gas slowly is poured in pyroreaction kettle, until mixed gas is discharged, the gas uses nitrogen；
Step 5, deposit, i.e. hydrophobic nano titanium dioxide will be obtained after pyroreaction kettle cooling pressure release.
Mass concentration of the tetrabutyl titanate in dehydrated alcohol in the step 1 is 50g/L, it is described stir evenly stir
Mixing speed is 1000r/min.
Mass concentration of the oleic acid in dehydrated alcohol in the step 2 is 50g/L, and the mixing speed stirred evenly is
500r/min。
The pressure of isothermal reaction in the step 2 is 0.3MPa, and temperature is 350 DEG C.
The pressure of isothermal reaction in the step 3 is 0.5MPa, and temperature is 360 DEG C.
The power of microwave reaction in the step 3 is 500W, and temperature is 400 DEG C, and the temperature of the constant temperature sedimentation is 350
℃。
The speed slowly poured in the step 4 is 50mL/min, and temperature is 330 DEG C.
Mixed gas in the step 4 can recycle to form oleic acid ethanol after cooling down, in step 2.
The cooling rate of cooling pressure release in the step 5 is 10 DEG C/min, and pressure release speed is 0.01MPa/min.
Through detecting, nano-titanium dioxide average-size is 450nm, and the thicknesses of layers of preparation is about 540nm, and water contact angle is
98.3 °, roll angle be 0.7 °.
Embodiment 2
A kind of preparation method of hydrophobic type titanium dioxide, includes the following steps:
Step 1, tetrabutyl titanate is added and is stirred evenly into dehydrated alcohol, obtain titanium alcohol liquid；
Step 2, oleic acid is added to absolute ethanol and is stirred evenly, isothermal reaction 4h is then added into pyroreaction kettle,
Obtain constant temperature atmosphere；
Step 3, isothermal reaction 5h in the pyroreaction kettle into step 2 is added in titanium alcohol liquid, then microwave reaction
150min, gas-solid mixture after constant temperature sedimentation；
Step 4, gas slowly is poured in pyroreaction kettle, until mixed gas is discharged, the gas uses inertia
Gas；
Step 5, deposit, i.e. hydrophobic nano titanium dioxide will be obtained after pyroreaction kettle cooling pressure release.
Mass concentration of the tetrabutyl titanate in dehydrated alcohol in the step 1 be 100g/L, described to stir evenly
Mixing speed is 2000r/min.
Mass concentration of the oleic acid in dehydrated alcohol in the step 2 is 100g/L, and the mixing speed stirred evenly is
1000r/min。
The pressure of isothermal reaction in the step 2 is 0.5MPa, and temperature is 370 DEG C.
The pressure of isothermal reaction in the step 3 is 0.7MPa, and temperature is 380 DEG C.
The power of microwave reaction in the step 3 is 800W, and temperature is 420 DEG C, and the temperature of the constant temperature sedimentation is 360
℃。
The speed slowly poured in the step 4 is 100mL/min, and temperature is 360 DEG C.
Mixed gas in the step 4 can recycle to form oleic acid ethanol after cooling down, in step 2.
The cooling rate of cooling pressure release in the step 5 is 20 DEG C/min, and pressure release speed is 0.02MPa/min.
Through detecting, nano-titanium dioxide average-size is 780nm, and the thicknesses of layers of preparation is about 450nm, and water contact angle is
111.1 °, roll angle be 0.6 °.
Embodiment 3
A kind of preparation method of hydrophobic type titanium dioxide, includes the following steps:
Step 1, tetrabutyl titanate is added and is stirred evenly into dehydrated alcohol, obtain titanium alcohol liquid；
Step 2, oleic acid is added to absolute ethanol and is stirred evenly, isothermal reaction 3h is then added into pyroreaction kettle,
Obtain constant temperature atmosphere；
Step 3, isothermal reaction 4h in the pyroreaction kettle into step 2 is added in titanium alcohol liquid, then microwave reaction
90min, gas-solid mixture after constant temperature sedimentation；
Step 4, gas slowly is poured in pyroreaction kettle, until mixed gas is discharged, the gas uses nitrogen
Or inert gas；
Step 5, deposit, i.e. hydrophobic nano titanium dioxide will be obtained after pyroreaction kettle cooling pressure release.
Mass concentration of the tetrabutyl titanate in dehydrated alcohol in the step 1 is 80g/L, it is described stir evenly stir
Mixing speed is 1500r/min.
Mass concentration of the oleic acid in dehydrated alcohol in the step 2 is 80g/L, and the mixing speed stirred evenly is
800r/min。
The pressure of isothermal reaction in the step 2 is 0.4MPa, and temperature is 360 DEG C.
The pressure of isothermal reaction in the step 3 is 0.6MPa, and temperature is 370 DEG C.
The power of microwave reaction in the step 3 is 700W, and temperature is 410 DEG C, and the temperature of the constant temperature sedimentation is 355
℃。
The speed slowly poured in the step 4 is 80mL/min, and temperature is 350 DEG C.
Mixed gas in the step 4 can recycle to form oleic acid ethanol after cooling down, in step 2.
The cooling rate of cooling pressure release in the step 5 is 15 DEG C/min, and pressure release speed is 0.02MPa/min.
Through detecting, nano-titanium dioxide average-size is 650nm, and the thicknesses of layers of preparation is about 500nm, and water contact angle is
108.1 °, roll angle be 0.7 °.
In conclusion the invention has the following advantages that
1. the present invention solves the problems such as prior art is at high cost, and process is complicated, the liquid of tetrabutyl titanate is hydrolyzed anti-
It should be converted into high temperature microwave vapor reaction, reduce reaction difficulty.
2. reaction system is converted vapor reaction by the present invention, it is ensured that the dispersibility of nanometer titanium dioxide forming, simultaneously
It is used without dispersing agent, reduces the generation of foreign gas.
3. the nano-titanium dioxide under the effect of hot kinetic energy is formed hydrophobic change with oleic acid gas using microwave reaction by the present invention
Property reaction, improve reaction efficiency, also solve oleic acid and tetrabutyl titanate under the conditions of liquid reacts difficulty.
4. present invention process is simple, exploitativeness is strong, and the exhaust gas mixing that simultaneous reactions generate can reuse, and reduces
The discharge of pollutant, meets national requirements for environmental protection.
It is understood that being merely to illustrate the present invention above with respect to specific descriptions of the invention and being not limited to this
Technical solution described in inventive embodiments.Those skilled in the art should understand that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technical effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (9)
1. a kind of preparation method of hydrophobic type titanium dioxide, characterized by the following steps:
Step 1, tetrabutyl titanate is added and is stirred evenly into dehydrated alcohol, obtain titanium alcohol liquid；
Step 2, oleic acid is added to absolute ethanol and is stirred evenly, isothermal reaction 2-4h is then added into pyroreaction kettle, obtains
To constant temperature atmosphere；
Step 3, isothermal reaction 2-5h in the pyroreaction kettle into step 2 is added in titanium alcohol liquid, then microwave reaction 30-
150min, gas-solid mixture after constant temperature sedimentation；
Step 4, gas slowly is poured in pyroreaction kettle, until mixed gas is discharged, the gas using nitrogen or
Inert gas；
Step 5, deposit, i.e. hydrophobic nano titanium dioxide will be obtained after pyroreaction kettle cooling pressure release.
2. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 1
Mass concentration of the tetrabutyl titanate in dehydrated alcohol be 50-100g/L, the mixing speed stirred evenly is 1000-
2000r/min。
3. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 2
Mass concentration of the oleic acid in dehydrated alcohol be 50-100g/L, the mixing speed stirred evenly is 500-1000r/min.
4. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 2
Isothermal reaction pressure be 0.3-0.5MPa, temperature be 350-370 DEG C.
5. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 3
Isothermal reaction pressure be 0.5-0.7MPa, temperature be 360-380 DEG C.
6. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 3
The power of microwave reaction be 500-800W, temperature is 400-420 DEG C, and the temperature of constant temperature sedimentation is 350-360 DEG C.
7. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 4
The speed slowly poured be 50-100mL/min, temperature be 330-360 DEG C.
8. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 4
Mixed gas can recycle to form oleic acid ethanol after cooling down, in step 2.
9. a kind of preparation method of hydrophobic type titanium dioxide according to claim 1, it is characterised in that: in the step 5
Cooling pressure release cooling rate be 10-20 DEG C/min, pressure release speed be 0.01-0.02MPa/min.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028359A (en) * | 2012-12-26 | 2013-04-10 | 内蒙古科技大学 | Microwave high-temperature chemical reaction system |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028359A (en) * | 2012-12-26 | 2013-04-10 | 内蒙古科技大学 | Microwave high-temperature chemical reaction system |
Non-Patent Citations (2)
| Title |
|---|
| 佚名: ""纳米钛白粉的制备法—钛醇盐气相水解法"", 《百度》 * |
| 刘成才主编: "《五邑大学优秀毕业论文集》", 30 April 2008, 华南理工大学出版社 * |
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Application publication date: 20190111 |