KR101625801B1 - Fabrication of Macroporous Titania Particles from Water-in-oil Emulsions And Macroporous Titania Particles - Google Patents

Fabrication of Macroporous Titania Particles from Water-in-oil Emulsions And Macroporous Titania Particles Download PDF

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KR101625801B1
KR101625801B1 KR1020150071925A KR20150071925A KR101625801B1 KR 101625801 B1 KR101625801 B1 KR 101625801B1 KR 1020150071925 A KR1020150071925 A KR 1020150071925A KR 20150071925 A KR20150071925 A KR 20150071925A KR 101625801 B1 KR101625801 B1 KR 101625801B1
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macropores
powder
porous
emulsion droplet
titania powder
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KR1020150071925A
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Korean (ko)
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조영상
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한국산업기술대학교산학협력단
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter

Abstract

Provided is a manufacturing method of a porous titania powder with macropores, which can synthesize the porous titania powder via a self-assembly process using emulsion. According to an embodiment of the present invention, the manufacturing method of a porous titania powder with macropores comprises the steps of: (a) emulsifying a polar solution composed of polymeric particles, a liquid precursor, water and hydrochloric acid in a nonpolar solution to form an emulsion droplet; (b) forming a composite powder composed of titania and the polymer particles via a self-assembly process while evaporating the polar solution in the emulsion droplet by heating the emulsion droplet; and (c) sintering the composite powder composed of titania and the polymer particles to remove the polymeric particle from the composite powder and form macropores, thereby forming the porous titania powder with macropores. In the step (a), the polar solution and the nonpolar solution are injected into a storage space of a rotating cylinder system which comprises an inner cylinder and an outer cylinder and has the storage space formed between the inner cylinder and the outer cylinder. In addition, when the outer cylinder is fixed and the inner cylinder is rotated, the polar solution is emulsified in the nonpolar solution by a vortex formed in the storage space so the emulsion droplet is formed.

Description

Technical Field [0001] The present invention relates to a method for producing a porous titania powder having macropores and a porous titania powder having macropores prepared therefrom,

TECHNICAL FIELD The present invention relates to a method for producing a porous titania powder having macropores and a porous titania powder having macropores prepared thereby. More specifically, the present invention relates to a method for producing a porous titania powder having large pores, )) To produce a porous titania powder having macropores capable of synthesizing a titania porous powder by a self-assembly technique utilizing an emulsion as a confined space, and a porous titania powder having macropores produced thereby .

Recently, the synthesis of porous materials for the application of photocatalysts, reflective pigments, phosphors, catalyst carriers, hydrogen generation and separation media has been extensively studied. Generally, porous materials refer to materials containing many pores.

Various synthetic routes such as a wet chemical method, a hydrothermal synthesis method, a colloidal casting method, a soft casting method and a hard casting method have been developed to synthesize a porous article. The soft-template method is a method in which an amphiphilic surfactant is self-assembled together with a precursor of a metal oxide, followed by high-temperature firing to remove the surfactant and form pores, It is a way to leave a skeletal structure. The hard-template method is a method of manufacturing a porous material having different materials by selectively impregnating pores in a porous metal oxide produced by a soft casting method with another material and then selectively removing only the metal oxide structure to be.

Among the various methods of producing high porosity materials, the colloidal casting method is a promising method because the pore size is easily controlled by adjusting the size of the template material. Accordingly, some developers have developed a colloidal casting method using various materials including nanoparticles dispersed or liquid precursor materials, but the technique of controlling the shape of the final porous body is a difficult problem in the field of colloid and interfacial engineering. In practical use, since the material having high porosity is advantageous, the shape of the porous body can be adjusted to a spherical shape or the like by using a fine droplet as a confined space.

According to a study by Velev et al., Porous particles with spherical shapes can be produced by utilizing droplets as a confined space, or other shapes can be manufactured with an external force such as an electric field. The synthesis of nanoparticles with porous structures can potentially be applied to sensors, sorbents and medical diagnostics.

In the past, inorganic nanostructures containing titania have been synthesized using a spray pyrolysis process with homogeneous macropores. Polystyrene latex particles as an artificial template material and inorganic nanoparticles as a precursor material were applied with a colloidal dispersion system.

Generally, in a spray dryer, a precursor material is supplied to a high-temperature reactor in the form of a fine droplet using a spray nozzle, and the aerosol is evaporated in a high-temperature reactor to induce self-assembly of the precursor. The calcination of the polymeric matrix material is performed in the same apparatus in a short cycle using a multi-stage reactor.

However, the spray pyrolysis method is disadvantageous in that the porous product is likely to adhere to the inner wall of the quartz tube inserted into the furnace at a high temperature, because evaporation of liquid droplets and decomposition of organic materials occur in one facility. This may act as a factor for lowering the yield of the porous powder synthesis process using the spray pyrolysis method, and it is required to synthesize the porous powder by applying a new process.

Besides the spray pyrolysis method, a self-assembly method using an emulsion can be considered, and a hydrophilic droplet can be used as a confined space for synthesis of porous particles. Instead of the dispersion of nanoparticles, a metal alkoxide such as titanium tetraisopropoxide (TTIP) is selected as a precursor material for synthesizing titania particles having macropores, and poly (meth) acrylates dispersed in hexane Methyl methacrylate microspheres have been selected as template materials for micrometer-sized macropores.

Unlike spray pyrolysis, this process requires the calcination process of self-assembled composite particles as a pre-stage to obtain porous particles without reducing the final product due to deposition in the quartz tube. However, when titanum tetraisopropoxide (TTIP) is used as a precursor material, it is possible to synthesize porous titania powder. However, since the TTIP is very sensitive to moisture in the air, reproducibility of experimental results may be deteriorated.

Korean Patent Laid-Open No. 10-2010-0021542 discloses a method for producing a silica-titania composite nanoporous material powder.

The present invention relates to a method for producing a titania porous powder which is capable of synthesizing a titania porous powder by using self-assembly technology using an emulsion as a limited space by utilizing TDIP (titanium diisopropoxide bis (acetylacetonate)) treated with acetylacetone as a precursor of a metal oxide And a method for producing the titania powder.

It is another object of the present invention to provide a method for producing a porous titania powder having macropores that can synthesize a porous powder having a macropore as a metal oxide material in addition to silica.

It is another object of the present invention to provide a method for producing porous titania powder having macropores capable of producing a porous powder having macropores that can be used as a photocatalyst for decomposing organic materials.

It is another object of the present invention to provide a method for producing porous titania powder having macropores capable of synthesizing a porous powder having macropores having a size within a range of several hundred nanometers to micrometers by performing dispersion polymerization.

According to an embodiment of the present invention, there is provided a method of preparing porous titania powder having macropores, comprising: (a) emulsifying a polar solution comprising polymer particles and a liquid precursor and water into a non-polar solution in which a surfactant is dissolved to form an emulsion droplet; (b) heating the emulsion droplet to form a composite powder of titania-polymer particles by self-assembly while volatile solvent and water contained in the emulsion droplet are evaporated; And (c) firing a composite powder of titania-polymer particles to remove macromolecule particles from the composite powder of titania-polymer particles to form macropores and to form porous titania powder having macropores, In the step (a), the polar solution and the nonpolar solution are introduced into a receiving space of a rotary cylinder system provided with an inner cylinder and an outer cylinder and having a receiving space between the inner cylinder and the outer cylinder, the outer cylinder is fixed, When rotated, it is preferable to emulsify by the vortex formed in the accommodation space to form an emulsion droplet.

In one embodiment of the present invention, the liquid precursor is preferably TDIP (titanium diisopropoxide bis (acetylacetonate)) treated with acetylacetone.

In one embodiment of the present invention, in step (b), the polar solution in the emulsion droplet is heated and evaporated while stirring slowly at 90 DEG C for 1 hour, and the calcination in step (c) .

delete

In one embodiment of the present invention, the emulsion droplets emulsified by the rotary cylinder system are formed by forming porous titania powder having macropores having a diameter in the range of 1 탆 to 18 탆 through steps (b) and (c) .

In one embodiment of the present invention, it is preferable that the titania powder having macropores has a diameter within a range of 1 탆 to 7 탆.

In one embodiment of the present invention, the nonpolar solution is an oil phase comprising hexadecane, and the oil phase is preferably a continuous phase.

In one embodiment of the present invention, the polymer particles are polystyrene particles formed by dispersion polymerization, and the polystyrene particles are preferably a template material for forming macropores in the composite powder after firing in the step (c).

Meanwhile, it is preferable that the porous titania powder having macropores according to an embodiment of the present invention is manufactured by a method of producing porous titania powder having macropores.

The present invention can synthesize the titania porous powder by self-assembly technique utilizing emulsion as a limited space by utilizing TDIP (titanium diisopropoxide bis (acetylacetonate)) treated with acetylacetone as a precursor material of metal oxide.

In addition, the present invention can synthesize a porous powder having macropores as a metal oxide material in addition to silica by utilizing titanium aceticacetonate (TDIP) treated with acetylacetone as a liquid precursor.

In addition, the present invention can be used for water treatment by using a porous powder having macropores as a photocatalyst for decomposing an organic material.

Disclosed is a method for producing porous titania powder having macropores capable of synthesizing a porous powder having macropores having a size ranging from several hundred nanometers to micrometers by performing dispersion polymerization.

In addition, the present invention can be manufactured by self-assembling a titania material having ultraviolet shielding properties with a micrometer-sized porous powder, thereby forming an ultraviolet blocking material free from the risk of human harm.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view of a process of synthesizing porous titania powder from polystyrene particles and a titania precursor by self-assembly using an emulsion liquid as a confining space, according to an embodiment of the present invention. FIG.
2 (a) is a scanning electron microscope image (with a scale bar of 3 m) of monodispersed polystyrene particles having a diameter of 640 nm synthesized by dispersion polymerization, and Fig. 2 (b) 2 (c) shows a scanning electron microscope image (the scale bar is 1 m) of the polystyrene particles having a diameter of 230 nm, and Fig. 2 (d) shows the particle size distribution of Fig. 2 (c).
3 (a) shows a scanning electron microscope image (scale bar of 10 m) of porous titania powder having macropores synthesized by using polystyrene particles having a diameter of 640 nm, and Fig. 3 (b) A scanning electron microscope image (with a scale bar of 3 m) of porous titania powder having macropores synthesized using polystyrene nanospheres having an average particle size of 3 nm is shown.
3 (c) shows a transmission electron microscope image (scale bar of 2 m) of the porous titania powder having macropores, and Fig. 3 (d) shows a transmission electron microscope image of the porous titania powder having macropores Are shown.
4 (b) is a graph showing the results of x-ray diffraction of the porous titania powder having macropores, and Fig. 4 (c) is a graph showing the results of x-ray diffraction of the porous titania powder having macropores. ) Schematically shows ultraviolet-visible light transmittance of porous titania powder having macropores.
5 is a schematic view of a process for producing porous titania powder having macropores using a rotary cylinder system.
Fig. 6 (a) shows a scanning electron microscope image of a porous titania powder having macropores produced using a rotating cylinder system, wherein the scanning electron microscope image has a scale bar of 50 m. FIG. 6 (b) shows a graph of particle size distribution of porous titania powder having macropores produced using a rotating cylinder system.
FIG. 7 is a schematic view showing a configuration used for a photocatalyst test using a porous titania powder having macropores.
FIG. 8A is a graph of rhodamine B concentration (C / C 0 ) according to UV irradiation time, FIG. 8B is a graph of change in rhodamine B concentration (C / C 0) Fig. 3 is a graph schematically showing a graph. Fig.

Hereinafter, with reference to the accompanying drawings, a method for manufacturing a porous titania powder having a macropore according to a preferred embodiment of the present invention and a porous titania powder having a macropore using the same will be described.

Hereinafter, with reference to the accompanying drawings, a method of manufacturing porous titania powder having macropores according to a preferred embodiment of the present invention and a porous titania powder 100b having macropores using the same will be described.

As shown in FIG. 1, a method of manufacturing porous pore-forming porous titania powder according to an embodiment of the present invention includes the steps of: (a) mixing polymer particles 101, a liquid precursor 103, water, ethanol, The polar liquid solution is emulsified in the nonpolar liquid to form the emulsion liquid droplet 100 and the polar liquid solution is evaporated in the emulsion liquid droplet 100 by the heating of the emulsion liquid droplet 100 in step (b) After the composite powder 100a of the titania-polymer particles 101 is formed, the composite powder 100a of the titania-polymer particles 101 is fired in the step (c), and the composite powder 100a of the titania- 100a, the macromolecule particles 101 are removed, and macropores are formed, so that the porous titania powder 100b having macropores can be produced.

As the polymer particles 101 shown in Fig. 1 (a), polystyrene particles synthesized by dispersion polymerization can be used. The polystyrene particles have a diameter of 230 nm to 640 nm. The process for synthesizing polystyrene nanospheres by dispersion polymerization is as follows.

Ethanol is fed into a batch reactor (not shown). The temperature of the batch reactor is maintained at 70 占 폚. Ethanol is used as a reaction solvent in which polyvinylpyrrolidone (PVP) is dissolved. The appropriate amount of styrene and MTC aqueous solution is then added to the batch reactor stirred at 170 rpm to 200 rpm.

Before the addition of an initiator, the operation of adding nitrogen to the reactor to remove oxygen is performed for 1.5 hours. An initiator is then added to the polymerization reactor to initiate particle synthesis and the reaction is continued for 19 hours.

In this embodiment, the porous titania powder having macropores is synthesized by using the polystyrene latex particles synthesized by the above process, and the synthesis is as follows.

Since the synthesized polystyrene latex particles contain a small amount of water, the polystyrene latex particles are redispersed in pure ethanol. To this end, an excess of ethanol is added to the colloidal dispersion of polystyrene before centrifugation. After centrifugation, only precipitated particles are collected, ethanol is added, and latex particles are redispersed in ethanol by ultrasonic waves. The final concentration of polystyrene particles in ethanol is approximately 30 wt%.

In this embodiment, the polar solution is formed by mixing polystyrene latex particles of polymer particles (101), liquid precursor (103), water and ethanol with a small amount of hydrochloric acid. The liquid precursor 103 may be titanium diisopropoxide bis (acetylacetonate) (TDIP) which is treated so as not to react sensitively with moisture in the air by acetylacetone.

That is, the polar solution was mixed with 30 wt% polystyrene particles dispersed in ethanol (7.5 g) and 0.01 N hydrochloric acid solution (1.6874 g) while stirring for 30 minutes, and then 3.25 g of TDIP was stirred for 1 hour and added dropwise Respectively. Then, to make the polar solution a dispersed phase, 4.268 g of water was added to the solution of TDIP and polystyrene latex and stirred for 30 minutes. In this embodiment, the polar solution corresponds to a dispersed phase.

Next, in order to form the emulsion droplet 100, the polar solution is emulsified in the nonpolar solution 104. Here, the nonpolar solution 104 may be an oil phase such as hexadecane having a concentration of 3 wt%. The non-polar solution 104 is a continuous phase.

The emulsification of the polar solution and the non-polar solution 104 is as follows. First, the nonpolar solution 104, which is a continuous phase, is added to the polar solution as a dispersed phase at a volume ratio of 1: 3, and an emulsion stabilizer (for example, ABIL EM90) is mixed with the nonpolar solution 104 and the polar solution. Thereafter, the non-polar solution 104 and the polar solution are mechanically emulsified for 60 seconds by using an emulsifier (homogenizer, not shown) to form an emulsion droplet 100 containing polystyrene latex particles .

Images of polystyrene particles formed by dispersion polymerization are shown in Figs. 2 (a) and 2 (c). 2 (a) is a scanning electron microscope image of monodisperse polystyrene particles having a diameter of 640 nm synthesized by dispersion polymerization when the scale bar is 3 m, and the image shown in Fig. 2 (c) Scanning electron microscope image showing polystyrene particles having a diameter of 230 nm when the bar is 1 m. Fig. 2 (b) is a graph showing the particle size distribution of monodispersed polystyrene particles having a diameter of 640 nm synthesized by dispersion polymerization. Fig. 2 (d) shows the particle size distribution of polystyrene particles having a diameter of 230 nm A graph is shown.

On the other hand, when the emulsion droplet 100 is formed by the above process, the evaporation of the emulsion droplet 100 is performed as shown in FIG. 1 (b).

Evaporation of the emulsion droplet 100 is carried out by heating at 90 DEG C for 1 hour while stirring the droplet. In the evaporation process of the emulsion droplet 100, volatile components such as ethanol in the emulsion droplet 100 and moisture are removed. In this exotherm, the liquid precursor 103 undergoes a sol-gel reaction to form a micrometer-sized metal oxide substrate 105). The metal oxide substrate may be formed into a spherical shape as shown in Fig. 1 (b), but is not necessarily limited to a spherical shape.

When the evaporation step of the emulsion droplet 100 is completed, a composite powder 100a comprising polystyrene particles and a metal oxide substrate is formed. The polystyrene particles are used as a template material for forming the macropores 108 after the firing process of the composite powder 100a.

In the next step, the composite powder 100a is sintered as shown in Fig. 1 (c) to form a porous titania powder 100b having macropores. When the composite powder 100a is fired, the polystyrene particles contained in the composite powder 100a are removed. Here, the firing process is performed for 5 hours in a box furnace operating at a temperature of 500 ° C. The polystyrene particles are removed from the composite powder 100a while being burned during the firing process, and macropores 108 are formed in the place where the polystyrene particles were present.

The porous titania powder 100b having macropores formed by the above process is as shown in FIG.

3 (a) shows a scanning electron microscope image of a porous titania powder 100b having macropores synthesized using polystyrene particles having a diameter of 640 nm when the scale bar is 10 m, and Fig. 3 (b) A scanning electron microscope image of a porous titania powder 100b having macropores synthesized by using polystyrene particles having a diameter of 640 nm when the scale bar is 3 mu m is shown. 3 (c) shows a transmission electron microscope image of the porous titania powder 100b having macropores when the scale bar is 2 占 퐉. In Fig. 3 (d), when the scale bar is 1 占 퐉, Is a transmission electron microscope image of the porous titania powder 100b having the porous titania powder 100b.

Fig. 4 (a) schematically shows a particle size distribution graph of the porous titania powder having macropores. As shown in Fig. 4 (a), the titania powder having macropores has a diameter within a range of 1 탆 to 7 탆, and the average diameter thereof is 2.99 탆. The titania powder having a large pore size prepared according to an embodiment of the present invention is micrometer-sized rather than nano-sized. It is large in size than the titania nanoparticles, and is difficult to penetrate into human skin. Even if it is inhaled into the respiratory tract, Can be manufactured from an ultraviolet shielding material which is free from the risk of human harm.

Fig. 4 (b) is a graph showing the results of x-ray diffraction of porous titania powder having macropores. FIG. 4 (b) shows the crystalline phase of the titania porous powder having macropores produced by mechanical emulsification through x-ray diffraction analysis, and it can be confirmed from the position of the diffraction peak that it has an anatase crystal structure.

On the other hand, FIG. 4 (c) shows a graph of ultraviolet-visible light transmittance of the porous titania powder having macropores. As shown in Fig. 4 (c), ultraviolet absorption occurs within a wavelength range of 260 nm to 320 nm, because the ultraviolet blocking degree of the titanic material is minimized in this range.

Hereinafter, with reference to FIGS. 5 and 6, a description will be given of the formation of the emulsion droplet 100 using the rotating cylinder system 10, rather than the emulsifier (homogenizer) generally used for mechanical emulsification . Here, FIG. 5 is a schematic view of a manufacturing process of porous titania powder having macropores using a rotary cylinder system.

As shown in Fig. 5 (a), the rotating cylinder system 10 includes an inner cylinder 11 and an outer cylinder 12. The inner cylinder 11 and the outer cylinder 12 have a structure rotatable with respect to each other. Between the inner cylinder 11 and the outer cylinder 12, a space 13 for accommodating the polar solution and the non-polar solution 104 is provided.

The polar solution and the nonpolar solution 104 contained in the accommodation space 13 are emulsified by the vortex generated in the accommodation space 13 so that the emulsion droplets (100). In addition to the process of producing the emulsion droplet 100, the evaporation process and the firing process of the emulsion droplet 100 are the same as those described above, so that a description thereof will be omitted in order to avoid repetition of the description.

6 (a) shows a scanning electron microscope image of a porous titania powder 100b having macropores produced using a rotating cylinder system 10, wherein the scanning electron microscope image has a scale bar of 50 占 퐉. 6 (b) shows a graph of the particle size distribution of the porous titania powder 100b having macropores produced using the rotating cylinder system 10. As shown in FIG. As shown in Fig. 6 (b), the diameter of the porous titania powder 100b having macropores is in the range of 1 탆 to 18 탆, and the average diameter is 4.45 탆.

The average diameter of the porous titania powder 100b having the large pores by forming the emulsion droplet 100 using a general emulsifier (not shown) is 2.99 mu m, while using the rotating cylinder system 10 The average diameter of the porous titania powder 100b having macropores obtained by forming the emulsion droplet 100 by evaporation and firing is 4.45 占 퐉 and the average diameter of the emulsion droplet 100 is measured using an emulsifier (homogenizer, not shown) The porous titania powder 100b having larger macropores can be produced when the emulsion droplets 100 are formed using the rotary cylinder system 10 rather than when forming the emulsion droplets 100. [

Hereinafter, with reference to FIGS. 7 and 8, the effect of using a titania powder having a large pore as a photocatalyst will be described. FIG. 7 schematically shows a configuration diagram used in a photocatalyst test by the porous titania powder 100b having macropores.

The porous titania powder 100b having macropores can be used as a photocatalyst for decomposing an organic material and can be used for water treatment. The photocatalytic test process using the porous titania powder 100b having macropores is as follows.

Prior to the photocatalytic test, a water soluble rhodamine B solution is prepared at a concentration of 0.002 g / L, and a water soluble rhodamine B solution is diluted in distilled water to control the concentration. The porous titania powder 100b having macropores is dissolved in distilled water at a concentration of 0.0001 g / L and mixed in a water-soluble rhodamine B solution at a volume ratio of 1: 1 to form a test solution 60. Prior to UV irradiation, test solution 60 is mixed for 30 minutes in a dark environment for equilibration.

As shown in FIG. 7, four UV lamps 70 are positioned so as to surround the test solution 60. UV lamps are used for photocatalytic reactions within a wavelength range of 352 nm to 369 nm. During the reaction, the UV lamp 70 and the test solution 60 are covered with a dark room 50 to prevent photodecomposition due to interference of external light.

Measurement of the UV absorbance is performed at regular time intervals. The initial concentration of rhodamine B in the mixed solution is determined by measuring the UV absorbance at 554 nm for 30 minutes in a dark room after equilibration. Figure 8 (a) is in the rhodamine B concentration (C / C 0) 8 graph, and also for the function (b) the rhodamine B concentration of the UV irradiation time (C / C 0) change with UV exposure time And a logarithmic function.

In FIG. 8 (a), C 0 is the initial concentration of the soluble rhodamine B solution, and C is the concentration after the equilibration of the aqueous rhodamine B solution. The slope shown in Fig. 8 (a) shows the slope of the decomposition rate. As the photocatalytic decomposition reaction is a primary reaction, the concentration of the water soluble rhodamine B decreases with increasing ultraviolet irradiation time.

The water soluble rhodamine B solution contains organic matter. The water-soluble rhodamine B solution is reddish in the initial state without photodegradation, and then the titania powder having macropores is introduced. When the ultraviolet ray is irradiated, the titania powder having macropores acts as a photocatalyst, .

The graph of FIG. 8 (b) is a logarithmic graph of the concentration change of the water soluble rhodamine B solution, where the slope represents the rate constant of the degradation reaction.

According to the graph shown in FIG. 8 (b), it can be seen that the rate at which the concentration of the water-soluble rhodamine B is reduced is proportional to the concentration depending on the ultraviolet irradiation time. Thus, when the reaction rate constant is large, It can be seen that it is decomposed quickly. That is, the porous titania powder 100b having macropores can decompose the water-soluble rhodamine B faster than the nanocrystals of spherical titania having a nanometer size.

Accordingly, it can be seen that the porous titania powder 100b having macropores can decompose organic substances more efficiently than nanometer sized titania microcrystals. As a result, the porous titania powder 100b having macropores can be used for a more efficient water treatment process.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be apparent to those of ordinary skill in the art.

100b: Porous titania powder having macropores
100: Emulsion droplet 100a: Composite powder
101: polymer particle 103: liquid precursor
104: nonpolar solution 105: metal oxide substrate
108: Giant pore

Claims (9)

(a) emulsifying a polar liquid composed of polymer particles, a liquid precursor, water and hydrochloric acid into a nonpolar solution to form an emulsion droplet;
(b) heating the emulsion droplet to form a composite powder of titania-polymer particles by self-assembly while the polar solution contained in the emulsion droplet is evaporated; And
(c) firing the composite powder of the titania-polymer particles to remove the polymer particles from the composite powder of the titania-polymer particles to form macropores, and forming the porous titania powder having the macropores and,
In the step (a), the polar solution and the non-
An internal combustion engine having an internal cylinder and an external cylinder, the internal cylinder being placed in the receiving space of a rotating cylinder system provided with a receiving space between the internal cylinder and the external cylinder,
Wherein when the outer cylinder is fixed and the inner cylinder is rotated, the emulsion droplet is emulsified by a vortex formed in the receiving space to form the emulsion droplet.
The method according to claim 1,
Wherein the liquid precursor is a mixture of titanium diisopropoxide bis (acetylacetonate) (TDIP) treated with acetylacetone.
The method according to claim 1,
In the step (b), the polar solution in the emulsion droplet is heated and evaporated while slowly stirring at 90 DEG C for 1 hour,
Wherein the calcination in step (c) is performed at 500 < 0 > C for 5 hours.
delete The method according to claim 1,
Wherein the emulsion droplet emulsified by the rotating cylinder system forms the porous titania powder having the macropores having a diameter in the range of 1 탆 to 18 탆 through the step (b) and the step (c) Wherein the porous titania powder has a large pore size.
The method according to claim 1,
Wherein the porous titania powder having macropores has a diameter within a range of 1 占 퐉 to 7 占 퐉.
The method according to claim 1,
Wherein the nonpolar solution is an oil phase comprising hexadecane and the oil phase is a continuous phase. ≪ RTI ID = 0.0 > 11. < / RTI >
The method according to claim 1,
The polymer particles are polystyrene particles formed by dispersion polymerization,
Wherein the polystyrene particles are a template material for forming the macropores in the composite powder after the firing in the step (c). ≪ RTI ID = 0.0 > 11. < / RTI >
A porous titania powder having macropores, which is produced by the method for producing a porous titania powder having the macropores of any one of claims 1 to 3 or 5 to 8.
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WO2019209071A1 (en) * 2018-04-26 2019-10-31 ㈜아모레퍼시픽 Method for manufacturing porous inorganic particle and light-reflecting composition comprising porous inorganic particle
US11390530B2 (en) 2017-06-02 2022-07-19 Amorepacific Cornoration Method for preparing porous inorganic particles

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JP2006116461A (en) * 2004-10-22 2006-05-11 Jsr Corp Laminate having visible light photocatalyst layer and visible light photocatalyst coating film
JP2006347826A (en) 2005-06-17 2006-12-28 National Institute For Materials Science Rare-earth element-doped titanium dioxide particle and its manufacturing method

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JP2006116461A (en) * 2004-10-22 2006-05-11 Jsr Corp Laminate having visible light photocatalyst layer and visible light photocatalyst coating film
JP2006347826A (en) 2005-06-17 2006-12-28 National Institute For Materials Science Rare-earth element-doped titanium dioxide particle and its manufacturing method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11390530B2 (en) 2017-06-02 2022-07-19 Amorepacific Cornoration Method for preparing porous inorganic particles
WO2019209071A1 (en) * 2018-04-26 2019-10-31 ㈜아모레퍼시픽 Method for manufacturing porous inorganic particle and light-reflecting composition comprising porous inorganic particle

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