KR101278047B1 - Manufacturing method for platinum dispersed tio2 precursor - Google Patents
Manufacturing method for platinum dispersed tio2 precursor Download PDFInfo
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- KR101278047B1 KR101278047B1 KR1020100130854A KR20100130854A KR101278047B1 KR 101278047 B1 KR101278047 B1 KR 101278047B1 KR 1020100130854 A KR1020100130854 A KR 1020100130854A KR 20100130854 A KR20100130854 A KR 20100130854A KR 101278047 B1 KR101278047 B1 KR 101278047B1
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Abstract
The present invention relates to a method of manufacturing a titanium dioxide precursor in which platinum is dispersed. A platinum-titanium precursor is prepared by mixing platinum added with methanol to a mixture of titanium added with methanol and L-lysine added with methanol. Preparing (Pt-Ti Precursor); Refluxing the platinum-titanium precursor; Preparing a platinum-titanium precursor solution by inducing a hydrolysis reaction by adding water to the refluxed platinum-titanium precursor; Titanium dioxide sol (TiO 2 ) in the platinum-titanium precursor solution and sol) to prepare a sol for producing nanofibers.
Thereby, a bond between platinum (Pt) and titanium (Ti), which is not chemically bonded, is reacted by adding L-lysine, which is a chemical binder, to prepare a platinum-titanium precursor primarily, and the platinum- By producing nanofibers using a nanofiber sol in which titanium dioxide sol is added to a titanium precursor, it is possible to produce good quality nanofibers while achieving uniform platinum dispersion and continuous, smooth and bead-free.
Description
The present invention relates to a method for preparing a titanium dioxide precursor in which platinum is dispersed, and more particularly, L-lysine (L-lysine), which is a chemical binder to bond between platinum (Pt) and titanium (Ti), which are not chemically bonded. Reaction was added to prepare a platinum-titanium precursor primarily, and nanofibers were prepared by using a nanofiber sol for which titanium dioxide sol was added to the platinum-titanium precursor, thereby achieving uniform platinum dispersion and continuous The present invention relates to a method for producing a platinum dispersed titanium dioxide precursor that can produce nanofibers of good quality that are soft and bead free.
Titanium dioxide (TiO 2 ) is a material that has been used for a long time in various fields because it is chemically inert, stable against chemical corrosion, and has the largest and cheapest photooxidation activity, and its application field is a catalyst, photocatalyst, dye sensitization. Various types of solar cells (electrode materials), sensors, and cosmetics.
However, the material used in most practical steps is complicated to manufacture by wet method using an oxide precursor in the form of nano powder or nanoparticles, and must be subjected to heat treatment at a high temperature of 700 to 800 ° C. or higher.
On the other hand, even in the case of coating the nano powder using a substrate, there are problems such as complicated manufacturing process, high manufacturing cost, and efficiency deterioration, and it is difficult to commercialize the air purification process due to processability and adhesion, and difficulty in recovery after catalytic reaction in water treatment process. There is this.
Recently, as a method for producing titanium dioxide nanofibers, which have attracted much attention, it can be obtained by electrospinning from a solution containing a precursor such as titanium salt or Ti (IV) -alkoxide.
However, since the fiber structure is greatly influenced by the compatibility of the titanium oxide precursor and the polymer contained in the spinning solution discharged from the spinneret with the polymer, the gelation reaction, and the concentration during electrospinning, it is difficult to manufacture nanofibers of equal quality. there was.
Therefore, the development of a method for producing a titanium dioxide precursor capable of obtaining uniform, good quality nanofibers, which is continuous, smooth and free of beads, has emerged.
The present invention was made to solve the above problems, and an object of the present invention is to add L-lysine, which is a chemical binder, to bond between platinum (Pt) and titanium (Ti), which are not chemically bound. To prepare a platinum-titanium precursor primarily, and to prepare nanofibers using a nanofiber sol in which a titanium dioxide sol is added to the platinum-titanium precursor, to realize uniform platinum dispersion and to be continuous and smooth. The present invention provides a method for producing a platinum-dispersed titanium dioxide precursor capable of producing good quality nanofibers without beads.
According to the present invention, a platinum-titanium precursor (Pt-Ti Precursor) is prepared by mixing platinum added with methanol to a mixture of methanol-added titanium and L-Lysine added with methanol. Making a step; Refluxing the platinum-titanium precursor; Preparing a platinum-titanium precursor solution by inducing a hydrolysis reaction by adding water to the refluxed platinum-titanium precursor; Titanium dioxide sol (TiO 2 ) in the platinum-titanium precursor solution It can be achieved by a method for producing a titanium dioxide precursor is dispersed in the platinum consisting of;
Here, in the step of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the platinum is added to the mixture of methanol and L- lysine (L-Lysine) added to the methanol, the methanol The added titanium may be prepared by adding methanol to a titanium diisopropoxide bis (acetylactonate) solution.
In addition, in the step of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the methanol is added to the mixture of the methanol and L- lysine (L-Lysine) to which the methanol is added, the methanol The added platinum may be prepared by adding methanol to a hydrogen hexachlorophatinate (IV) hexahydrate solution.
In addition, in the step of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the methanol is added to the mixture of the methanol and L- lysine (L-Lysine) to which the methanol is added, the methanol The added titanium is 6 to 10 parts by weight (wt%), methanol is added L- lysine is 11 to 13 parts (wt%), methanol is added to 25 to 30 parts by weight (wt%) Can be.
On the other hand, refluxing the platinum-titanium precursor (reflux) is a step of refluxing the platinum-titanium precursor at 120 ~ 240 (min) at 60 ~ 90 (℃).
Here, the step of preparing a platinum-titanium precursor solution by inducing a hydrolysis reaction by adding water to the refluxed platinum-titanium precursor, 60 ~ 90 (℃) the platinum-titanium precursor solution to which distilled water is added Reflux step at 900 ~ 1020 (min).
In addition, a titanium dioxide sol (TiO 2 ) in the platinum-titanium precursor solution In the step of preparing a sol for manufacturing nanofibers by adding a sol), the titanium dioxide sol may be prepared by mixing titanium (IV) tetraisopropoxide and polyvinylpyrrolidone.
Here, the titanium salt is prepared to have a concentration of 0.14g / mL by mixing 1.5g of titanium, 3mL of ethanol and 3mL of glacial acetic acid, the polyvinylpyrrolidone, 0.675g of PVP and 7.5mL of ethanol The mixture is prepared to have a PVP concentration of 0.09 g / mL, and the titanium dioxide sol is prepared by mixing the titanium salt and polyvinylpyrrolidone.
In addition, a titanium dioxide sol (TiO 2 ) in the platinum-titanium precursor solution sol) is added to prepare a sol for preparing nanofibers, and a 3 mL platinum-titanium precursor solution and the titanium dioxide sol are synthesized to prepare a sol for preparing nanofibers.
Here, the method of manufacturing the titanium dioxide precursor in which the platinum is dispersed, further comprises the step of heat-treating the sol for producing nanofibers at 120 ~ 240 (min) at 450 ~ 600 (℃).
According to the present invention, a bond between platinum (Pt) and titanium (Ti), which is not chemically bonded, is reacted by adding L-lysine, a chemical binder, to prepare a platinum-titanium precursor. By producing nanofibers using a nanofiber sol with a titanium dioxide sol added to a platinum-titanium precursor, it is possible to produce good quality nanofibers with uniform platinum dispersion and continuous, smooth and bead free. have.
BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.
1 is a flow chart of a method for producing a titanium dioxide precursor in which platinum is dispersed according to the present invention,
FIG. 2 is a graph showing an XRD (X-ray Diffraction) analysis result of a nanofiber sol prepared by a method for preparing a platinum dispersed titanium dioxide precursor according to the present invention.
FIG. 3 is a SEM analysis result of a nanofiber sol prepared by the method for preparing a titanium dioxide precursor in which platinum is dispersed according to the present invention, (a) is an image of a sol for nanofiber manufacturing before heat treatment, and (b) is Image of a sol for making nanofibers.
Hereinafter, the configuration of the present invention will be described in detail with reference to the accompanying drawings.
Prior to this, the terms used in the specification and claims should not be construed in a dictionary sense, and the inventor may, on the principle that the concept of a term can be properly defined in order to explain its invention in the best way And should be construed in light of the meanings and concepts consistent with the technical idea of the present invention.
Therefore, the embodiments shown in the present specification and the drawings are only exemplary embodiments of the present invention, and not all of the technical ideas of the present invention are presented. Therefore, various equivalents It should be understood that water and variations may exist.
1 is a flow chart of a method for producing a platinum dispersed titanium dioxide precursor according to the present invention, Figure 2 is a XRD (X-X) of a sol for preparing nanofibers prepared by the method for producing a titanium dioxide precursor dispersed in platinum ray Diffraction) is a graph of the analysis results, Figure 3 is a SEM analysis result of the nanofiber sol prepared by the method for producing a titanium dioxide precursor dispersed in platinum according to the present invention, (a) is a sol for nanofiber manufacturing before heat treatment (B) is an image of a sol for preparing nanofibers after heat treatment.
1 to 3, according to the present invention, a method for preparing a platinum dispersed titanium dioxide precursor according to the present invention includes adding methanol to a mixture of titanium added with methanol and L-lysine added with methanol. Mixing platinum to prepare a platinum-titanium precursor (Pt-Ti Precursor) (S10); Refluxing the platinum-titanium precursor (S20); Adding a water to the refluxed platinum-titanium precursor to induce a hydrolysis reaction to prepare a platinum-titanium precursor solution (S30); Titanium dioxide sol (TiO 2 ) in the platinum-titanium precursor solution sol) is added to prepare a sol for manufacturing nanofibers (S40).
Here, in the step (S10) of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the methanol added platinum to the mixture of the methanol and L- lysine (L-Lysine) is added methanol The titanium added with methanol may be prepared by adding methanol to a titanium diisopropoxide bis (acetylactonate) solution.
Preferably, the methanol is added to titanium, may be prepared by adding 3.64g of titanium diisopropoxide bis (acetylactonate) solution to 60mL of methanol.
In addition, L-lysine to which the methanol is added may be prepared by adding 0.179 g of L-lysine to 20 mL of methanol.
In addition, the platinum to which methanol is added may be prepared by adding 0.433 g of hydrogen hexachloropetinate hexahydrate solution to 20 mL of methanol.
Here, the platinum-titanium precursor may be prepared by mixing the platinum solution added with methanol in a state where the titanium added with methanol and L-lysine added with methanol are mixed first.
In addition, in the step (S10) of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the methanol added platinum to the mixture of the methanol and L- lysine (L-Lysine) is added methanol The platinum-titanium precursor is 6-10 parts by weight (wt%) of titanium to which methanol is added, 11-13 parts by weight (wt%) of L-lysine to which methanol is added and platinum to 25 is added to methanol. It may be formulated at a rate of ˜30 parts by weight (wt%).
After the platinum-titanium precursor prepared as described above is subjected to a reflux step (S20), water is added to induce a hydrolysis reaction (S30), and then titanium dioxide sol is added (S40), and heat treatment (S50). The nanofiber sol is finally finished.
Here, the step of refluxing the platinum-titanium precursor (S20) is a step of refluxing the platinum-titanium precursor at 120 to 240 (min) at 60 to 90 (° C.), preferably the platinum to The titanium precursor is refluxed at 80 ° C. for 180 min.
Subsequently, adding a water to the refluxed platinum-titanium precursor to induce a hydrolysis reaction (S30) to prepare a platinum-titanium precursor solution, 60 ~ 90 distilled water added platinum-titanium precursor solution Refluxing at (° C.) for 900 to 1020 (min), preferably, by refluxing the platinum-titanium precursor solution to which distilled water is added at 80 ° C. for 960 (min), whereby the platinum-titanium precursor solution is 1 It is completed sequentially.
Here, by synthesizing the titanium dioxide sol to be described later in the platinum-titanium precursor solution, the sol for producing nanofibers according to the present invention is finally completed, the manufacturing process of the titanium dioxide sol will be described in detail.
The titanium dioxide sol may be prepared by mixing titanium (IV) tetraisopropoxide and polyvinylpyrrolidone.
Here, the titanium salt is prepared to have a concentration of 0.14g / mL by mixing 1.5g of titanium, 3mL of ethanol and 3mL of glacial acetic acid, the polyvinylpyrrolidone, 0.675g of PVP and 7.5mL of ethanol Are mixed to provide a PVP concentration of 0.09 g / mL.
That is, the titanium dioxide sol is completed by mixing the titanium salt and polyvinylpyrrolidone prepared as described above.
Here, the nano-fiber sol is the titanium dioxide sol (TiO 2 in the above-described platinum-titanium precursor solution sol) is added, and preferably, 3 mL of a platinum-titanium precursor solution and a titanium dioxide sol having the same concentration and weight are synthesized to finally prepare a sol for producing nanofibers.
Here, the method for producing a titanium dioxide precursor in which platinum is dispersed according to the present invention further includes the step (S50) of the nanofiber manufacturing sol being heat treated at 450 to 600 (° C.) for 120 to 240 (min).
Subsequently, the sol for manufacturing nanofibers may be processed into nanofibers through heat treatment and electrospinning processes.
Here, the nanofiber sol prepared by the method described above, the surface tension was 21.4 (mN / m), the viscosity showed 16.6 (cP), as shown in Figure 2, XRD results, platinum (Pt) It can be confirmed that the anatase titanium dioxide is uniformly dispersed and distributed on the matrix.
In addition, as shown in Figure 3 (a), (b), the diameter of the nanofibers before the heat treatment (a) was approximately 430 (nm), the diameter of the nanofibers after the heat treatment (b) was observed to 150 (nm).
As described above, according to the present invention, a method for preparing a titanium dioxide precursor in which platinum is dispersed is obtained by using L-lysine, which is a chemical binder, to form a bond between platinum (Pt) and titanium (Ti) that are not chemically bonded. By adding and reacting to prepare a platinum-titanium precursor primarily, and by preparing a nanofiber using a nanofiber manufacturing sol in which a titanium dioxide sol is added to the platinum-titanium precursor, even platinum dispersion is realized and at the same time continuous It can produce good quality nanofibers that are soft and bead free.
As mentioned above, although the present invention has been described by way of limited embodiments and drawings, the technical idea of the present invention is not limited thereto, and a person having ordinary skill in the art to which the present invention pertains, Various modifications and variations may be made without departing from the scope of the appended claims.
Claims (10)
Refluxing the platinum-titanium precursor;
Preparing a platinum-titanium precursor solution by inducing a hydrolysis reaction by adding water to the refluxed platinum-titanium precursor;
And adding a titanium dioxide sol (TiO 2 sol) to the platinum-titanium precursor solution to prepare a sol for producing nanofibers.
In the step of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the methanol added platinum to a mixture of the methanol added L-Lysine (L-Lysine) and methanol added, the methanol is added Titanium is prepared by adding methanol to a solution of titanium diisopropoxide bis (acetylactonate),
In the step of preparing a platinum-titanium precursor (Pt-Ti Precursor) by mixing the methanol added platinum to a mixture of the methanol added L-Lysine (L-Lysine) and methanol added, the methanol is added The prepared platinum is a method for producing a platinum dispersed titanium dioxide precursor, characterized in that methanol is added to a hydrogen hexachlorophatinate (IV) hexahydrate solution.
Refluxing the platinum-titanium precursor is a step of refluxing the platinum-titanium precursor at 60 to 90 ° C. for 120 to 240 min, wherein the platinum-titanium precursor is dispersed. Manufacturing method.
Inducing the hydrolysis reaction by adding water to the refluxed platinum-titanium precursor to prepare a platinum-titanium precursor solution, the platinum-titanium precursor solution to which distilled water is added 900 to 60 ~ 90 (℃) Platinum-dispersed titanium dioxide precursor, characterized in that the step of reflux for ~ 1020 (min).
The titanium dioxide sol is a titanium salt (Titanium (IV) tetraisopropoxide) and polyvinylpyrrolidone (Polyvinylpyrrolidone) in the step of preparing a sol for manufacturing nanofibers by adding a titanium dioxide sol (TiO 2 sol) to the platinum-titanium precursor solution Method for producing a titanium dioxide precursor dispersed platinum is characterized in that the mixture is provided.
The titanium salt is 1.5 g of titanium, 3 mL of ethanol and 3 mL of glacial acetic acid is prepared to have a concentration of 0.14 g / mL, the polyvinyl pyrrolidone, 0.675 g of PVP and 7.5 mL of ethanol is mixed It is provided to have a PVP concentration of 0.09g / mL, the method of producing a platinum dispersed titanium dioxide precursor, characterized in that the titanium dioxide sol is provided by mixing the titanium salt and polyvinylpyrrolidone.
In the preparing of the nanofiber sol by adding a titanium dioxide sol (TiO 2 sol) to the platinum-titanium precursor solution, 3mL of the platinum-titanium precursor solution and the titanium dioxide sol are synthesized to prepare a sol for nanofiber manufacturing Method for producing a platinum dispersed titanium dioxide precursor, characterized in that the step.
The method of manufacturing the titanium dioxide precursor in which the platinum is dispersed, further comprises the step of heat-treating the sol for manufacturing the nanofiber at 450 to 600 (° C.) for 120 to 240 (min). Method for preparing a precursor.
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| US6645902B2 (en) | 2000-05-15 | 2003-11-11 | Ngk Insulators, Ltd. | Adsorbent having capability of decomposing organic halogen compounds and method for producing the same |
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| US6645902B2 (en) | 2000-05-15 | 2003-11-11 | Ngk Insulators, Ltd. | Adsorbent having capability of decomposing organic halogen compounds and method for producing the same |
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