KR20170043865A - MANUFACTURING METHOD OF TiO2 FLOWER SPHERE-REDUCED GRAPHENE OXIDE COMPOSITES - Google Patents
MANUFACTURING METHOD OF TiO2 FLOWER SPHERE-REDUCED GRAPHENE OXIDE COMPOSITES Download PDFInfo
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- KR20170043865A KR20170043865A KR1020150143479A KR20150143479A KR20170043865A KR 20170043865 A KR20170043865 A KR 20170043865A KR 1020150143479 A KR1020150143479 A KR 1020150143479A KR 20150143479 A KR20150143479 A KR 20150143479A KR 20170043865 A KR20170043865 A KR 20170043865A
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- C01B31/043—
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The present invention provides a new waste water treatment complex by a method for producing a complex of flower-like spherical TiO 2 and reduced graphene oxide which can be used for treatment of refractory organic matter in the field of wastewater treatment. The present invention relates to (1) oxidation of graphite Preparing graphene oxide that has been stripped by the reaction; (2) thermally synthesizing tetrabutyl titanate (TBT) and acetic acid to produce flower-like spherical TiO 2 ; (3) hydrothermally synthesizing the graphene oxide prepared in the step (1) and the flower-like spherical TiO 2 prepared in the step (2); And (4) drying the hydrothermally synthesized sample in the step (3).
According to the present invention, since the flower spherical TiO 2 has high light absorption, excellent pore structure and reduced energy level of reduced graphene oxide, it is possible to produce a composite having greatly improved optical activity.
Description
The present invention is to provide a new wastewater treatment complex through a process for producing a complex of a flower-like spherical TiO 2 and reduced graphene oxide which can be used for treatment of a refractory organic matter in the field of wastewater treatment.
Recently, rapid growth of science and industry, environmental pollution, and population increase have caused pollution and depletion of water resources. Since such water pollution can not be solved by natural circulation, it is urgent to study environmentally friendly and practical wastewater treatment. On the other hand, waste water treatment technologies include electrolysis, adsorption, absorption, and redox reaction of a photocatalyst. Particularly, a photocatalytic wastewater treatment technology is environmentally friendly and has excellent regeneration. In particular, TiO 2 is attracting attention because it is eco-friendly, economical, chemically, biologically and thermodynamically very stable. However, since TiO 2 can only absorb light in a short wavelength range corresponding to the ultraviolet region, it has a disadvantage that it can not absorb a visible light region occupying a large range of solar energy, and commercially developed TiO 2 is easy to recover There is a disadvantage that a means for preventing recombination of electron-hole pairs is required continuously.
An object of the present invention is to provide a wastewater treatment complex having hydrolysis efficiency of organic matter decomposition efficiency by hydrothermal synthesis of flower-like spherical TiO 2 and graphene oxide.
According to one aspect of the present invention, there is provided a method for preparing a flower-shaped spherical TiO 2 -reduced graphene oxide composite, comprising the steps of: (1) preparing graphene oxide which has been peeled off by oxidation of graphite; (2) thermally synthesizing tetrabutyl titanate (TBT) and acetic acid to produce flower-like spherical TiO 2 ; (3) hydrothermally synthesizing the graphene oxide prepared in the step (1) and the flower-like spherical TiO 2 prepared in the step (2); And (4) drying the hydrothermally synthesized sample in the step (3).
In the step (1), the oxidation reaction is performed in a mixed solution of sulfuric acid and phosphoric acid, and the sulfuric acid and phosphoric acid may be in a volume ratio of 1: 9 to 10: 0.
In the step (2), the solvent thermo-synthesis may be carried out at 120 to 300 ° C for 4 to 24 hours.
In step (2), the flower-like spherical TiO 2 produced through solvent thermo-synthesis may be fired at 300 to 900 ° C for 1 to 6 hours.
In step (3), the content of graphene oxide may be 0.1 to 30 parts by weight based on 100 parts by weight of spherical spherical TiO 2 .
In the step (3), hydrothermal synthesis may be performed at 120 to 300 ° C for 1 to 24 hours.
In accordance with the present invention as described above, the separation by oxidation of graphite graphene oxide and by a flower-shaped spherical TiO 2 prepared by the solvothermal synthesis hydrothermal synthesis, flower-shaped spherical TiO 2 - to prepare a reduced graphene oxide composite There is an effect that can be.
In addition, according to the present invention, since the flower spherical TiO 2 has high light absorption, excellent pore structure and reduced energy level of reduced graphene oxide, it is possible to produce a composite having greatly improved optical activity, Has a low band gap, a low electron-hole pair recombination ratio, and a photocatalyst characteristic even in the visible light region, and thus can be applied to various fields such as materials for advanced water treatment, semiconductors, and solar cells.
Figure 1 is a SEM photograph of the graphene oxide composite with a reduced flower-shaped spherical TiO 2 manufactured by the manufacturing method according to an aspect of the present invention.
FIG. 2 is a TEM photograph of a flower-shaped spherical TiO 2 and a reduced graphene oxide composite prepared by the manufacturing method according to an embodiment of the present invention.
FIG. 3 is a graph showing a rhodamine B decomposition curve of a flower-shaped spherical TiO 2 and a reduced graphene oxide complex produced by a manufacturing method according to an embodiment of the present invention, according to irradiation time of visible light.
Hereinafter, the present invention will be described in detail.
A method for preparing a flower-like spherical TiO 2 -reduced graphene oxide complex according to an embodiment of the present invention comprises the steps of: (1) preparing graphene oxide peeled by oxidation of graphite; (2) thermally synthesizing tetrabutyl titanate (TBT) and acetic acid to produce flower-like spherical TiO 2 ; (3) hydrothermally synthesizing the graphene oxide prepared in the step (1) and the flower-like spherical TiO 2 prepared in the step (2); And (4) drying the hydrothermally synthesized sample in the step (3).
In the step (1), the oxidation reaction may be performed by adding potassium permanganate in a mixed solution of sulfuric acid and phosphoric acid. The sulfuric acid and phosphoric acid may be mixed in a volume ratio of 1: 9 to 10: 1, and more preferably, the mixing ratio of sulfuric acid and phosphoric acid may be 5: 5 to 9.5: 0.5. On the other hand, if the volume ratio of sulfuric acid is less than 1, the oxidation reaction is insignificant. If the volume ratio is more than 9.5, the structure of graphite may be destroyed.
The step (1) is a step of oxidizing graphite to prepare graphene oxide. The graphite may be added to a mixed solution of sulfuric acid and phosphoric acid together with potassium permanganate and reacted at 50 ° C for 24 hours to prepare a mixture. The mixture is washed with hydrochloric acid, ethanol and distilled water in this order, and then freeze-dried in a freeze dryer at -70 to 0 ° C for 48 to 300 hours To produce graphene oxide. If the freeze-drying temperature is less than -70 ° C, the freeze-drying effect is insignificant. If the freeze-drying time is less than 48 hours, the freeze-drying effect is insignificant. If the freeze- Lt; / RTI >
The step (2) is a step of preparing a flower-shaped spherical TiO 2 photocatalyst, wherein the TBT and the acetic acid can be mixed in a volume ratio of 1:15 to 1:85. When the volume ratio of acetic acid is less than 15, synthesis is not carried out in the form of a flower when the solvent is thermally synthesized. When the volume ratio is more than 85, The mixture of TBT and acetic acid may be subjected to a solvent thermal synthesis reaction at 120 to 300 ° C for 4 to 24 hours to prepare flower-shaped spherical TiO 2 . If the solvent thermosynthesis temperature is less than 120 ° C, the synthesis is not carried out. If the solvent temperature is more than 300 ° C, the TiO 2 shape is deformed when the solvent is thermally synthesized. If the solvent thermosetting time is less than 4 hours, the synthesis is not carried out, and if it exceeds 24 hours, the TiO 2 shape is deformed.
In addition, the step (2) may include a step of drying the solution at 60 to 120 ° C for 6 to 24 hours after the heat-synthesis reaction. When the temperature is lower than 60 ° C, drying is not performed. If it exceeds 120 ° C, the sample is damaged. If it is less than 6 hours, it will not be dried. If it exceeds 24 hours, it will damage the sample.
The step (2) may further include a step of baking the produced flower-shaped spherical TiO 2 at 300 to 900 ° C for 1 to 6 hours under air atmosphere. The calcination effect is insignificant when calcined at a temperature less than 300 ° C, and the specimen is damaged when the calcination temperature exceeds 900 ° C. The calcination effect is insignificant when calcined in less than 1 hour, and the sample is deformed and damaged in case exceeding 6 hours.
The step (3) is a step of preparing a flower-like spherical TiO 2 -reduced graphene oxide complex, wherein the content of the graphene oxide may be 0.1 to 30 parts by weight based on 100 parts by weight of the spherical spherical TiO 2 . If the content of the graphene oxide is less than 0.1 part by weight, the photocatalytic synergistic effect is insignificant. When the content of the graphene oxide is more than 30 parts by weight, clumping of graphene oxide occurs. The step (3) may be performed in distilled water, and hydrothermal synthesis may be performed at 120 to 300 ° C for 1 to 24 hours. If the hydrothermal synthesis temperature is lower than 120 ° C, the synthesis is not carried out. If the hydrothermal synthesis temperature is higher than 300 ° C, the reduced graphene oxide structure is destroyed. The graphene oxide is converted into reduced graphene oxide while performing the hydrothermal synthesis reaction.
The step (4) is a step of recovering the spherical TiO 2 -reduced graphene oxide by drying the hydrothermally synthesized sample in the step (3), and centrifuging at 5000 to 8000 rpm, To < / RTI > 24 hours. When centrifuged at 5000 rpm or less, centrifugation is not carried out, and when it exceeds 8000 rpm, sample damage is caused. If drying is not carried out at a temperature lower than 60 ° C during drying, and if it is higher than 120 ° C, damage to the sample is caused. Also, if the drying time is less than 6 hours, it will not be dried, and if it exceeds 24 hours, the sample will be damaged.
Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these examples are for illustrative purposes only and that the scope of the present invention is not construed as being limited by these examples.
Example 1.
3 g of graphite and 18 g of potassium permanganate are added to a mixed solution of sulfuric acid and phosphoric acid in a volume ratio of 5: 5, reacted at 50 ° C for 24 hours, and then put in a mixed solution of 3 ml of hydrogen peroxide and ice water. The filtered samples were washed with hydrochloric acid, ethanol and distilled water in this order, and then freeze-dried at -70 ° C for 96 hours using a freeze dryer for drying to prepare graphene oxide. Next, 15 mL acetic acid is mixed with 1.5 mL TBT and stirred for 10 minutes. This was added to a Teflon-line autoclave and thermally synthesized at 120 ° C for 6 hours, washed twice with ethanol, and then dried at 80 ° C for 12 hours. Thereafter, the calcined TiO 2 photocatalyst was sintered at 300 ° C for 1 hour under an air atmosphere to prepare a flower-shaped spherical TiO 2 photocatalyst. 0.15 g of flower-shaped spherical TiO 2 and 0.1 part of graphene oxide were added to 50 ml of distilled water, and 0.1 part of graphene oxide was added to 100 parts by weight of spherical TiO 2. The mixture was stirred for 30 minutes and then stirred in a Teflon-line autoclave for hydrothermal synthesis To prepare a suspension in the form of a suspension. Finally, the suspended suspension is centrifuged at 8000 rpm for 10 minutes using a centrifuge and dried at 80 ° C for 12 hours to prepare a flower-shaped spherical TiO 2 -reduced graphene oxide complex.
Example 2.
The procedure of Example 1 was repeated except that the volume of acetic acid was changed to 30 mL, the heat reaction temperature of the solvent was set to 150 ° C, the sintering temperature was set to 400 ° C, and the prepared spherical TiO 2 and graphene oxide Stirred for 60 minutes, and hydrothermally synthesized for 2 hours to prepare a flower-shaped spherical TiO 2 -reduced graphene oxide complex.
Example 3.
The procedure of Example 2 was repeated except that the volume ratio of sulfuric acid to phosphoric acid was 7: 3, the volume of acetic acid was 45 mL, the content of graphene oxide was 0.5 part by weight based on 100 parts by weight of spherical spherical TiO 2 , The complex was hydrothermally synthesized at a temperature of 150 ℃ for 4 hours to prepare a flower - like spherical TiO 2 - reduced graphene oxide complex.
Example 4.
The same procedure as in Example 3 was carried out except that the volume of acetic acid was changed to 75 mL, the solvent heat reaction temperature was set to 180 ° C, and the sintering temperature was set to 500 ° C. During the preparation of the composite, spherical TiO 2 and graphene oxide The time is 120 minutes and hydrothermal synthesis is carried out for 6 hours to prepare flower-shaped spherical TiO 2 -reduced graphene oxide complex.
Example 5.
The procedure of Example 4 was repeated except that the volume ratio of sulfuric acid and phosphoric acid was set to 9: 1, the firing time was set to 2 hours, the content of graphene oxide was changed to 1 part by weight based on 100 parts by weight of spherical spherical TiO 2 , And hydrothermal synthesis is carried out at 180 ° C in the preparation of the composite to prepare a flower-like spherical TiO 2 -reduced graphene oxide complex.
Example 6.
The procedure was carried out in the same manner as in Example 5 except that the volume ratio of sulfuric acid and phosphoric acid was set to 10: 0, the solvent heat reaction temperature was set to 210 ° C, the sintering was performed at a sintering temperature of 700 ° C for 4 hours, flower-shaped and spherical TiO 2 100 parts of 3 weight parts by weight of the preparation, the composite after the manufacture of flower-shaped spherical TiO 2 and the graphene oxide was stirred for 150 minutes by synthetic sequence for 12 h at 210 ℃ flower-shaped spherical TiO 2 - reduced To prepare a graphene oxide complex.
Example 7.
The synthesis was carried out the above described process in the same manner as in Example 6, the volume ratio of sulfuric acid and phosphoric acid 3: and 7, and a solvothermal reaction temperature at 250 ℃, complex manufacturing Yes pins oxide content flower-shaped spherical TiO 2 100 parts by weight And the hydrothermal synthesis was carried out for 18 hours with stirring time of the spherical TiO 2 powder and the graphene oxide for 180 minutes to prepare a flower spherical TiO 2 -reduced graphene oxide complex.
Example 8.
The procedure of Example 7 was followed except that the volume of acetic acid was changed to 85 mL and the mixture was calcined at 800 ° C for 6 hours. The graphene oxide content in the preparation of the composite was changed from 20 to 100 parts by weight of spherical TiO 2 And the stirring time is 210 minutes. Hydrothermal synthesis is performed at 300 ° C to prepare a flower-like spherical TiO 2 -reduced graphene oxide complex.
Example 9.
The procedure of Example 8 was repeated except that the volume ratio of sulfuric acid and phosphoric acid was 1: 9, the solvent thermal reaction was performed at 300 ° C, the sintering temperature was 900 ° C, and the content of graphene oxide spherical shape, and TiO 2 100 parts by
Comparative Example 1
The procedure of Example 5 was followed except that no solvent thermal reaction was carried out and a flower spherical TiO 2 photocatalyst was prepared without graphene oxide.
Comparative Example 2
The process is carried out in the same manner as in Example 5, except that a flower-like spherical TiO 2 photocatalyst is prepared without graphene oxide.
Measurement example 1. The flower-like spherical TiO 2 prepared in the present invention 2 - Observation of morphology and surface structure of reduced graphene oxide complex
The morphology and surface structure of the floral spherical TiO 2 -reduced graphene oxide complex prepared by the present invention were observed through Scanning Electron Microscopy (SU8010, Hitach Co., LTD).
Measurement example 2: The flower-like spherical TiO 2 - Observation of morphology and surface structure of reduced graphene oxide complex
The morphology and surface structure of the flower-shaped spherical TiO 2 -reduced graphene oxide complex prepared in the present invention were observed through a Transmission Electron Microscope (TEM-2100F, JEOL Co., USA).
Measurement Example 3 [0042] The flower-like spherical TiO 2 - Determination of photodegradation ability of reduced graphene oxide complex
A solar simulator (Model 11000, Abet Technologies, USA) was installed for agitation with solar irradiation to measure the photodegradation ability of spherical TiO 2 -reduced graphene oxide complexes, and the reactor was equipped with a 70 mL vial bottle And 0.02 g of the flower-shaped spherical TiO 2 -reduced graphene oxide complex was added to 50 ml of 15 ppm rhodamine B (rhodamine B). First, the flower - shaped spherical TiO 2 - reduced graphene oxide complex was stabilized with rhodamine solution for 30 minutes in the dark room condition where no external light was applied, and then photodegraded by stirring with sunlight.
A UV-Vis spectrophotometer (S-3100, Scinco Co., Korea) was used to measure photodegradation rate, and samples were taken at 15-minute intervals for 2 hours.
(h)
Having described specific portions of the present invention in detail, those skilled in the art will appreciate that these specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereby. something to do. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (6)
(2) thermally synthesizing tetrabutyl titanate (TBT) and acetic acid to produce flower-like spherical TiO 2 ;
(3) hydrothermally synthesizing the graphene oxide prepared in the step (1) and the flower-like spherical TiO 2 prepared in the step (2); And
(4) drying the sample hydrothermally synthesized in the step (3)
Wherein the grained TiO 2 -doped graphene oxide complex is formed by a method comprising the steps of:
In the step (1), the oxidation reaction is performed in a mixed solution of sulfuric acid and phosphoric acid, and the sulfuric acid and phosphoric acid are in a volume ratio of 1: 9 to 10: 0. The spherical TiO 2 -reduced graphene oxide complex ≪ / RTI >
The method of the reduced graphene oxide composite-flower shape spherical TiO 2, characterized in that for performing the above (2) solvothermal synthesis in step is from 120 to 300 ℃ for 4 to 24 hours.
Wherein the step (2) comprises calcining the flower-shaped spherical TiO 2 produced through solvent thermo-synthesis at 300 to 900 ° C for 1 to 6 hours. The method for producing the flower-shaped spherical TiO 2 -reduced graphene oxide composite .
The above-mentioned (3) The content of the oxide pins Yes in step is flower-shaped spherical TiO flower-shaped spherical TiO 2, characterized in that 2100 parts by weight of 0.1 to 30, based on the weight of the-method of the reduced graphene oxide composite.
The 3 step is flower-shaped spherical TiO 2, characterized in that performing the random number sequence from 1 to 24 hours during synthesis at 120 to 300 ℃ - production method of the reduced graphene oxide composite.
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| CN108686592A (en) * | 2018-05-21 | 2018-10-23 | 陕西科技大学 | A kind of preparation method of sea urchin shape bivalve layer hollow microsphere |
| CN108751168A (en) * | 2018-06-08 | 2018-11-06 | 常州大学盱眙凹土研发中心 | A kind of preparation method of the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type for photoproduction cathodic protection |
| WO2019085532A1 (en) * | 2017-11-01 | 2019-05-09 | 南通纺织丝绸产业技术研究院 | Composite material of trivalent titanium self-doped titanium dioxide nanoparticles-partially reduced graphene oxide nanosheets and preparation method therefor |
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| KR101414539B1 (en) * | 2013-05-22 | 2014-07-04 | 인하대학교 산학협력단 | METHOD OF PRODUCING GRAPHENE/TiO2 COMPOSITES |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019085532A1 (en) * | 2017-11-01 | 2019-05-09 | 南通纺织丝绸产业技术研究院 | Composite material of trivalent titanium self-doped titanium dioxide nanoparticles-partially reduced graphene oxide nanosheets and preparation method therefor |
| CN108686592A (en) * | 2018-05-21 | 2018-10-23 | 陕西科技大学 | A kind of preparation method of sea urchin shape bivalve layer hollow microsphere |
| CN108686592B (en) * | 2018-05-21 | 2020-11-13 | 陕西科技大学 | Preparation method of sea urchin-shaped double-shell hollow microspheres |
| CN108751168A (en) * | 2018-06-08 | 2018-11-06 | 常州大学盱眙凹土研发中心 | A kind of preparation method of the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type for photoproduction cathodic protection |
| CN108751168B (en) * | 2018-06-08 | 2020-10-30 | 常州大学盱眙凹土研发中心 | Preparation method of anatase type flower-like rhombic titanium dioxide/graphene composite material for photo-generated cathode corrosion prevention |
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