CN101062780A - Nano titanium oxide and mechanical force chemical reaction preparation method for its composite powder - Google Patents
Nano titanium oxide and mechanical force chemical reaction preparation method for its composite powder Download PDFInfo
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Abstract
The invention discloses a preparing technology of nanometer titanium oxide and composite powder body, which comprises the following steps: using shearing force and impact force generated in balling course to bruise solid phase reacting system; increasing specific surface area of the reactant; improving reaction rate to advance the ratio of nucleation rate and growth rate; preparing fine and even forerunner material; washing; drying; controlling the temperature and time of heat decomposition; getting nanometer titanium oxide and composite powder body with diverse crystal system and grain size; realizing surface coating of nanometer titanium oxide. This method possesses simple craft and can control crystal system, outlook and grain diameter of nanometer titanium oxide, which powder grain diameter distribution is 30-80nm.
Description
One, technical field
This patent of invention belongs to " nano oxide powder technology of preparing ", relates to a kind of nano titanium oxide in fields such as makeup, coating and preparation method of composite granule thereof of can be used for.
Two, background technology
Nano-TiO
2Because of safety, nontoxic, non-stimulated, safe and reliable, UVA, UVB are had excellent shielding effect, good stability, absorb do not decompose after the ultraviolet ray, nondiscoloration, therefore be widely used in ultraviolet shielded fields such as sun care preparations, exterior coating.At present normal powder and the film that adopts chemical processes such as physical method such as vapour deposition, sputter and sol-gel, hydro-thermal be synthetic to prepare nano titanium oxide.For example: application number is 200410022136.9, name is called the Chinese patent application of " a kind of preparation method of controllable size distribution gold redrock nano-titanium dioxide ", application number is 200310106562.6, name is called the Chinese patent application of " a kind of preparation method of rutile-phase nano-titanium dioxide ", application number is 03126532.4, name is called the Chinese patent application of " nano titanic oxide sol coating and method for making thereof and purposes ", application number is 01113393.7, name is called the Chinese patent application of " is that raw material low temperature prepares gold redrock nano-titanium dioxide with positive metatitanic acid ", and application number is 99116814.3, name is called the Chinese patent application of " a kind of preparation method of nano titanium oxide ";
From the content of above Chinese patent application as can be seen: these preparation method's required equipment complexity, its synthesis condition are comparatively harsh, and the production cycle is longer, thereby production cost is higher.In addition, in order to reduce the optical activity of nano titanium oxide, must carry out the surface to nano titanium oxide and coat processing, thereby increase subsequent treatment process.
Three, summary of the invention
The present invention is directed to the deficiency that prior art exists, the mechanical force and chemical reaction method of a kind of nano titanium oxide and composite granule thereof is provided, this kind method has not only been simplified technology, and prepared nano titanium dioxide crystal form, particle diameter, pattern are controlled; By adjusting reaction system and proportioning thereof, can in the preparation nano titanium oxide, generate mineral powders such as nano zine oxide, nano-aluminium oxide on its surface, realize in the preparation nano titanium oxide that promptly the surface coats.
Mechanism of the present invention is: utilize the shearing force that produces in the mechanical milling process, surging force can broken solid-phase reactant, increase the specific surface area of reactant, improve reactant contact surface and speed of reaction, therefore improved the ratio of nucleation rate and growth rate, can prepare fine, uniform precursor, control heat decomposition temperature and time then, thereby can obtain the nano titanium oxide and the composite granule thereof of different crystal forms, different-grain diameter, realize that simultaneously the surface of nano titanium oxide coats.
Method provided by the invention is a raw material with the complex body and the part thereof of single titaniferous reactant or titaniferous reactant and zinc salt or aluminium salt, and processing step is as follows successively:
1, batching
The mol ratio of reactant and part is 1: 2-6
2, batch mixing
The reactant and the part thereof that will meet ratio mix, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling, make under its mechanical shear stress that in mechanical milling process, produces, the impact force action reaction generate precursor, till reactant and its part fully chemical reaction take place;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities;
5, precursor drying
Precursor is dry to adopt natural air drying or oven dry under 30-80 ℃;
6, precursor thermolysis
The precursor heat decomposition temperature is controlled at 400-600 ℃, time is 2-4 hour, can obtain nanometer anatase titania, also can be at 300-500 ℃ of following pre-burning 0.5-1.5 hour, then 750-900 ℃ of decomposition, time is 1.5-4 hour, obtains rutile type nano titanic oxide or surface coated rutile type nano titanic oxide composite granule.
In the aforesaid method, reactant is the mixture of titaniferous reactants such as butyl (tetra) titanate, metatitanic acid, titanium sulfate or butyl (tetra) titanate, metatitanic acid, titanium sulfate and zinc sulfate (or zinc chloride), Tai-Ace S 150 (or aluminum chloride), and part is mainly oxalic acid, sodium oxalate, yellow soda ash, sodium bicarbonate, volatile salt or bicarbonate of ammonia etc.; The lubricant that is added during ball milling is ethanol or acetone.
The nano titanium oxide and the composite granule thereof of method preparation provided by the invention, powder size is distributed as 30-80nm, and its powder morphology can be regulated according to application need.
The present invention has the following advantages and beneficial effect:
1, owing to reacts under the effect of the shearing force that reaction system produces in mechanical milling process, surging force, can increase the specific surface area of reactant, the velocity of diffusion of particle in the contact surface of raising reactant and the system, thereby chemical reaction velocity is accelerated, cause nucleation rate to be far longer than the nuclear growth rate, chemical time shortens, and easily forms the precursor of fine particles, has created condition for obtaining nano-powder.
2, by adjusting thermal decomposition process, precursor can obtain the nano titanium oxide and the composite granule thereof of different crystal forms through thermolysis.
Four, description of drawings
Fig. 1 is a kind of process flow sheet according to the mechanical force chemical reaction preparation method of nano titanium oxide provided by the present invention and composite granule thereof.
Five, embodiment
Embodiment 1:
In the present embodiment, reactant is a butyl (tetra) titanate, and part is an oxalic acid, and technical process has following steps as shown in Figure 1 successively
1, batching
The mol ratio of butyl (tetra) titanate and oxalic acid is 1: 3
2, batch mixing
The butyl (tetra) titanate that will meet ratio mixes with oxalic acid, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The butyl (tetra) titanate and the oxalic acid that mix are carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is controlled at 300 rev/mins, and ball milling can make butyl (tetra) titanate and oxalic acid that chemical reaction takes place fully in 50 minutes and generate precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is an ethanol, washing and filtering three times;
5, precursor drying
Precursor after the removal of impurities is 40 ℃ of oven dry down, and the time is 6 hours;
6, precursor thermolysis
Precursor after the oven dry is placed resistance furnace or retort furnace, and heat decomposition temperature is controlled at 500 ℃, and the time is 2 hours, can obtain nanometer anatase titania;
Precursor after the oven dry is placed resistance furnace or retort furnace, and heat decomposition temperature is controlled at 800 ℃, and the time is 2 hours, obtains rutile type nano titanic oxide.
Embodiment 2:
In the present embodiment, reactant is a titanium sulfate, and part is a yellow soda ash, and technical process has following steps as shown in Figure 1 successively
1, batching
The mol ratio of titanium sulfate and yellow soda ash is 1: 4
2, batch mixing
The titanium sulfate that will meet ratio mixes with yellow soda ash, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The titanium sulfate and the yellow soda ash that mix are carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is at 320 rev/mins, and ball milling can make titanium sulfate and yellow soda ash that chemical reaction takes place fully in 40 minutes and generate precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is a distilled water, washing and filtering three times;
5, precursor drying
Precursor after the removal of impurities is 80 ℃ of oven dry down, and the time is 4 hours;
6, precursor thermolysis
Precursor after the oven dry is placed resistance furnace or retort furnace, and heat decomposition temperature is controlled at 550 ℃, and the time is 2 hours, can obtain nanometer anatase titania;
Precursor after the oven dry is placed resistance furnace or retort furnace, and heat decomposition temperature is controlled at 850 ℃, and the time is 2 hours, obtains rutile type nano titanic oxide.
Embodiment 3:
In the present embodiment, reactant is the complex body of titanium sulfate, zinc sulfate, and part is an oxalic acid, and technical process has following steps as shown in Figure 1 successively
1, batching
The complex body of titanium sulfate, zinc sulfate and the mol ratio of oxalic acid are 1: 3, and the mol ratio of titanium sulfate, zinc sulfate is 10: 1 in the complex body;
2, batch mixing
To meet the titanium sulfate of ratio, the complex body of zinc sulfate mixes with oxalic acid, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is at 250 rev/mins, and ball milling can make titanium sulfate, thin sour zinc and oxalic acid that chemical reaction takes place fully in 60 minutes and generate precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is a distilled water, washing and filtering twice, and then with washing with alcohol once;
5, precursor drying
Presoma after the removal of impurities is natural air drying at room temperature, and the time is 10 hours;
6, precursor thermolysis
Titanous oxalate after the oven dry is placed resistance furnace or retort furnace, heat decomposition temperature is controlled at 400 ℃, predecomposition 40 minutes, heat decomposition temperature is controlled at 800 ℃ then, time is 2 hours, obtain the composite granule of nano zine oxide and nm-class rutile-type TiO 2, the part nano zine oxide is coated on the surface of nano titanium oxide.
Embodiment 4
In the present embodiment, reactant is the complex body of metatitanic acid, Tai-Ace S 150, and part is a volatile salt, and technical process has following steps as shown in Figure 1 successively
1, batching
The complex body of metatitanic acid, Tai-Ace S 150 and the mol ratio of volatile salt are 1: 6, and the mol ratio of metatitanic acid, Tai-Ace S 150 is 12: 1 in the complex body;
2, batch mixing
To meet the metatitanic acid of ratio, the complex body of Tai-Ace S 150 mixes with volatile salt, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is at 230 rev/mins, ball milling can make the complex body of metatitanic acid, Tai-Ace S 150 and volatile salt that chemical reaction takes place fully in 80 minutes, generated precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is a distilled water, washing and filtering twice, and then with washing with acetone once;
5, precursor drying
Presoma after the removal of impurities is 50 ℃ of oven dry, and the time is 5 hours;
6, precursor thermolysis
Precursor after the oven dry is placed resistance furnace or retort furnace, heat decomposition temperature is controlled at 500 ℃, predecomposition 30 minutes, heat decomposition temperature is controlled at 800 ℃ then, time is 2.5 hours, obtain the composite granule of nano-aluminium oxide and nm-class rutile-type TiO 2, the part nano-aluminium oxide is coated on the surface of nano titanium oxide.
Embodiment 5:
In the present embodiment, reactant is the complex body of metatitanic acid, zinc chloride, and part is a bicarbonate of ammonia, and technical process has following steps as shown in Figure 1 successively
1, batching
The complex body of metatitanic acid, zinc chloride, with the mol ratio of bicarbonate of ammonia be 1: 5, the mol ratio of metatitanic acid, zinc chloride is 8: 1 in the complex body;
2, batch mixing
To meet the metatitanic acid of ratio, the complex body of zinc chloride, mix, till evenly with bicarbonate of ammonia;
3, the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is at 400 rev/mins, ball milling can make the complex body of metatitanic acid, zinc chloride and bicarbonate of ammonia that chemical reaction takes place fully in 30 minutes, generated precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is an ethanol, washing and filtering twice, and then with washing with acetone once;
5, precursor drying
Presoma after the removal of impurities is 60 ℃ of oven dry, and the time is 5 hours;
6, precursor thermolysis
Precursor after the oven dry is placed resistance furnace or retort furnace, heat decomposition temperature is controlled at 400 ℃, predecomposition 30 minutes, heat decomposition temperature is controlled at 750 ℃ then, time is 2.5 hours, obtain the composite granule of nano zine oxide and nm-class rutile-type TiO 2, the part nano zine oxide is coated on the surface of nano titanium oxide.
Embodiment 6:
In the present embodiment, reactant is the complex body of titanium sulfate, aluminum chloride, and part is a sodium bicarbonate, and technical process has following steps as shown in Figure 1 successively
1, batching
The complex body of titanium sulfate, aluminum chloride, with the mol ratio of sodium bicarbonate be 1: 5, the mol ratio of titanium sulfate, aluminum chloride is 13: 1 in the complex body;
2, batch mixing
To meet the titanium sulfate of ratio, the complex body of aluminum chloride mixes with sodium bicarbonate, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is at 450 rev/mins, ball milling can make the complex body of titanium sulfate, aluminum chloride and sodium bicarbonate that chemical reaction takes place fully in 30 minutes, generated precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is an ethanol, washing and filtering twice, and then with distilled water wash once;
5, precursor drying
Presoma after the removal of impurities is natural air drying at room temperature, and the time is 12 hours;
6, precursor thermolysis
Precursor after the oven dry is placed resistance furnace or retort furnace, heat decomposition temperature is controlled at 450 ℃, predecomposition 50 minutes, heat decomposition temperature is controlled at 850 ℃ then, time is 2 hours, obtain the composite granule of nano-aluminium oxide and nm-class rutile-type TiO 2, the part nano-aluminium oxide is coated on the surface of nano titanium oxide.
Embodiment 7:
In the present embodiment, reactant is the complex body of butyl (tetra) titanate, zinc chloride, and part is a sodium oxalate, and technical process has following steps as shown in Figure 1 successively
1, batching
The complex body of butyl (tetra) titanate, zinc chloride, with the mol ratio of sodium oxalate be 1: 2, the mol ratio of butyl (tetra) titanate, zinc chloride is 6: 1 in the complex body;
2, batch mixing
To meet the butyl (tetra) titanate of ratio, the complex body of zinc chloride mixes with sodium oxalate, till evenly;
3, the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling under room temperature, normal pressure, make reaction generation precursor under its mechanical shear stress that in mechanical milling process, produces, the impact force action, the rotating speed of ball mill is at 380 rev/mins, ball milling can make the complex body of butyl (tetra) titanate, zinc chloride and sodium oxalate that chemical reaction takes place fully in 40 minutes, generated precursor;
4, precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities, and washing composition is an acetone, washing and filtering twice, and then with washing with alcohol once;
5, precursor drying
Presoma after the removal of impurities is natural air drying at room temperature, and the time is 8 hours;
6, precursor thermolysis
Precursor after the oven dry is placed resistance furnace or retort furnace, heat decomposition temperature is controlled at 500 ℃, predecomposition 30 minutes, heat decomposition temperature is controlled at 900 ℃ then, time is 1.5 hours, obtain the composite granule of nano-aluminium oxide and nm-class rutile-type TiO 2, the part nano-aluminium oxide is coated on the surface of nano titanium oxide.
Claims (3)
1, the present invention relates to the preparation method of a kind of nano titanium oxide and composite granule thereof, it is characterized in that with titaniferous reactant and part thereof be raw material, technological process is as follows:
(1) batching
The mol ratio of reactant and part is 1: 2-6
(2) batch mixing
The reactant and the part thereof that will meet ratio mix, till evenly;
(3) the mechanical force and chemical reaction method prepares precursor
The reaction system that mixes is carried out ball milling, make under its mechanical shear stress that in mechanical milling process, produces, the impact force action reaction generate precursor, till reactant and its part fully chemical reaction take place;
(4) precursor removal of impurities
The washing and filtering method is adopted in the precursor removal of impurities;
(5) precursor drying
Precursor is dry to adopt natural air drying or oven dry under 30-80 ℃;
(6) precursor thermolysis
The precursor heat decomposition temperature is controlled at 400-600 ℃, time is 24 hours, can obtain nanometer anatase titania, also can be at 300-500 ℃ of following pre-burning 0.5-1.5 hour, then 750-900 ℃ of decomposition, time is 1.5-4 hour, obtains rutile type nano titanic oxide or surface coated rutile type nano titanic oxide composite granule.
2, the preparation method of nano titanium oxide according to claim 1 and composite granule thereof is characterized in that reactant is the mixture of titaniferous reactants such as butyl (tetra) titanate, metatitanic acid, titanium sulfate or butyl (tetra) titanate, metatitanic acid, titanium sulfate and zinc sulfate or zinc chloride, Tai-Ace S 150 or aluminum chloride.
3, the preparation method of nano titanium oxide according to claim 1 and 2 and composite granule thereof is characterized in that part is mainly oxalic acid, sodium oxalate, yellow soda ash, sodium bicarbonate, volatile salt or bicarbonate of ammonia etc.
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