KR101616088B1 - Manufacturing method attached silane functional group for hexagonal and cubic mesoporous silica materials at room temperature - Google Patents
Manufacturing method attached silane functional group for hexagonal and cubic mesoporous silica materials at room temperature Download PDFInfo
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- KR101616088B1 KR101616088B1 KR1020140078888A KR20140078888A KR101616088B1 KR 101616088 B1 KR101616088 B1 KR 101616088B1 KR 1020140078888 A KR1020140078888 A KR 1020140078888A KR 20140078888 A KR20140078888 A KR 20140078888A KR 101616088 B1 KR101616088 B1 KR 101616088B1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
Abstract
The present invention relates to a process for preparing a mesoporous silica material having silane functional groups, comprising the steps of: (a) mixing H 2 O and EtOH at a constant ratio; (b) adding a surfactant to the solution in which H 2 O and EtOH are mixed at a predetermined ratio; (c) adding a compound selected from the group consisting of a precursor of the mesoporous silica material and a silane functional group to the solution formed in step (b), and stirring the mixture at room temperature for a predetermined time; (d) adding ammonia water to the solution stirred in step (c) and stirring for a predetermined time; (e) washing and drying the material synthesized in the step (d) after filtration; And (f) firing after the step (e).
It is another object of the present invention to provide a method for producing a mesoporous silica material with a silane-based functional group attached thereto, thereby increasing the specific surface area of the mesoporous silica material and improving the adsorption capacity according to the structure. The carbon dioxide is chemically bonded by the carbon nanotubes, and the adsorption amount can be greatly increased.
Description
More particularly, the present invention relates to a method for producing a mesoporous silica material having a pore structure of a hexagonal structure and a cubic structure in a room temperature manufacturing process and having a silane-based functional group attached thereto.
The mesoporous material refers to a porous material having a nanometer size according to the definition of IUPAC (International Union of Pure and Applied Chemistry), and when the pore size is 2 nm or less depending on the pore size, microporous, (Mesoporous), and when they have pores of 50 nm or more, they are called macroporous. Porous materials with nanometer-sized pores can be used as a host or chromatographic separation of organic polymers when forming organic / inorganic composites, adsorption of toxic substances in air and water, and morphological selective catalysts of large organic polymers Much research has been done because of potential applicability.
The mesoporous material started in 1990 by T. Yanagisawa and his colleagues synthesized materials with uniform size pores ranging from 1.8 nm to 3.2 nm using the surfactant as a template. Subsequently, in 1992, J. S. Beck and others of Mobil synthesized hexagonal mesoporous materials and successfully synthesized mesoporous materials of cubic and lamellar structures.
The sol-gel method, which has been studied so far, reacts by heating at a high temperature during the condensation reaction, which complicates the process due to heating and increases the cost. Therefore, studies for conducting a condensation reaction at room temperature have been actively conducted. By adjusting the pH during the condensation reaction, the process can be simplified and the cost can be reduced.
To synthesize mesoporous materials, nonionic surfactants and cationic surfactants are used as supports. Synthesis of mesoporous material with the cationic surfactant of is no direct way of S + + I - → S + I - S + + X using the methods and media of synthesizing such as - + I + = S + X - I +. & Lt ; / RTI > Where S + is a cationic surfactant, I + and I - are inorganic ions, and X - is a mediating ion.
The cationic surfactant, which is mainly used in the synthesis of mesoporous materials, is the alkali ammonium halide (C n H 2n +1 N + X - ). When this surfactant is dissolved in a certain concentration in a solution, it forms a structure, which is called a critical micelle concentration. Depending on the surfactant concentration, hexagonal, cubic, and lamellar structures lamellar. FIG. 1 is a schematic diagram of the structure formation according to the critical micelle concentration and the synthesis of the mesoporous material. FIG.
Silane with amine groups at the carbon chain end was used to attach the amine group to the mesoporous silica material thus regulated. A simple schematic diagram of gas adsorption is shown in FIG.
When carbon dioxide or toxic gas, which is a greenhouse gas, passes through a silica material having a functional group in the atmosphere, the gases are chemically bonded selectively to a functional group on the surface of the silica material.
The adsorption of carbon dioxide on the amine group is shown in Fig. When the two amine groups on the surface of the mesoporous silica adsorbent meet with carbon dioxide, they are converted into carbamate and ammonium ions by oxidation-reduction reaction, and eventually converted into ion-bonded forms in which carbonate and ammonium ions are bonded. do.
The sol-gel method, which has been studied so far, reacts by heating at a high temperature during the condensation reaction, which complicates the process due to heating and increases the cost. In addition, the mesoporous silica material used as the adsorbent A method for producing a mesoporous silica material which can broaden the specific surface area by an efficient and simple process is needed in order to improve the adsorption performance.
The object of the present invention to solve the above problems is to synthesize a mesoporous silica material through a condensation reaction at room temperature, and to simplify the process and reduce the cost by synthesizing the mesoporous silica material by adjusting the pH during the condensation reaction.
The present invention also provides a method for improving the adsorption capacity depending on the structure by enlarging the specific surface area, and the mesoporous silica adsorbent having mesoporous silica adsorbent, which is capable of chemically bonding carbon dioxide by the functional group on the surface of the mesoporous silica adsorbent, And to provide a method for producing a substance.
According to an aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: (a) mixing H 2 O and EtOH at a predetermined ratio; (b) adding a surfactant to the solution in which H 2 O and EtOH are mixed at a predetermined ratio; (c) adding a compound selected from the group consisting of a precursor of the mesoporous silica material and a silane functional group to the solution formed in step (b), and stirring the mixture at room temperature for a predetermined time; (d) adding ammonia water to the solution stirred in step (c) and stirring for a predetermined time; (e) washing and drying the material synthesized in the step (d) after filtration; And (f) firing after the step (e).
In the step (b), it is preferable to add CTACl as the surfactant, and it is preferable that the concentration ratio of SiO 2 and CTACl Is preferably 0.1 to 0.2 in one unit.
Preferably, the pore structure of the silica material may have a hexagonal structure when the concentration ratio of SiO 2 to CTACl is in the range of 0.1 to less than 0.15, and the concentration ratio of SiO 2 to CTACl may be 0.15 to 0.15, 0.2 or less, the pore structure of the silica material may have a cubic structure.
In addition, it is preferable to add TEOS as the precursor in the step (c), and the molar concentration of the TEOS is in the range of 0.1 to 0.4 M, and the molar concentration is increased to increase the specific surface area of the silica material In step (d), it is preferable to add ammonia water so that the pH of the solution is set in the range of 9-11.
In a second aspect of the present invention, there is provided a method for producing a mesoporous silica material, comprising the steps of: synthesizing a mesoporous silica material to which the silane-based functional group is attached through a condensation reaction at room temperature, In the process of forming gel after forming the sol in the process, the mesoporous silica material is synthesized by setting the pH of the solution to 9 to 11 by adding the base solution at the room temperature.
Here, it is preferable that the cationic surfactant is a CTACl in the course of the synthesis of the silica material, to which a silane-based functional group is attached.
As described above, the present invention is advantageous in that the structure of the hexagonal structure and the cubic structure can be controlled and the mesoporous silica material having a large specific surface area can be synthesized using the ratio of the additive materials at room temperature.
In addition, the present invention can synthesize a mesoporous silica material through a condensation reaction at room temperature without heating process for supplying heat, and at this time, by adjusting the pH during the condensation reaction, the process can be simplified and cost can be reduced.
It is another object of the present invention to provide a method for producing a mesoporous silica material having a silane-based functional group, thereby providing a method of increasing the specific surface area and improving the adsorption capacity according to the structure, And the carbon dioxide is chemically bonded by the carbon nanotubes, thereby increasing the adsorption amount.
FIG. 1 is a schematic diagram of the structure formation according to the critical micelle concentration and the synthesis of the mesoporous material,
Fig. 2 is a simple schematic diagram for gas adsorption,
3 is a schematic view showing adsorption of carbon dioxide on an amine group,
4 is a view showing a flow of a process for producing a mesoporous silica material with a silane-based functional group according to an embodiment of the present invention,
FIG. 5 is a view showing the structure of aminosilane used in a method for producing a mesoporous silica material according to an embodiment of the present invention,
Figure 6 shows the XRD results of a mesoporous silica material with a functional group having a hexagonal pore structure,
Figure 7 shows the XRD results of a functionalized mesoporous silica material with a cubic pore structure,
Figure 8 is a TEM photograph of a hexagonal mesoporous silica material with amine groups,
9 is a TEM photograph of a cubic mesoporous silica material with amine groups,
10 is a graph of FT-IR results of mesoporous silica having an amine group as a hexagonal pore structure functional group,
11 is a graph of the FT-IR results of mesoporous silica having amine groups attached to the functional group of a cube pore structure.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and how to accomplish it, will be described with reference to the embodiments described in detail below with reference to the accompanying drawings. However, the present invention is not limited to the embodiments described herein but may be embodied in other forms. The embodiments are provided so that those skilled in the art can easily carry out the technical idea of the present invention to those skilled in the art.
In the drawings, embodiments of the present invention are not limited to the specific forms shown and are exaggerated for clarity. Also, the same reference numerals denote the same components throughout the specification.
The expression "and / or" is used herein to mean including at least one of the elements listed before and after. Also, singular forms include plural forms unless the context clearly dictates otherwise. Also, components, steps, operations and elements referred to in the specification as " comprises "or" comprising " refer to the presence or addition of one or more other components, steps, operations, elements, and / or devices.
Hereinafter, preferred embodiments according to the present invention will be described in detail with reference to the drawings.
FIG. 4 is a flow chart of a method for producing a mesoporous silica material with a silane-based functional group according to an embodiment of the present invention, and FIG. 5 is a cross-sectional view illustrating a method of manufacturing a mesoporous silica material according to an embodiment of the present invention Aminosilane < / RTI >
As shown in FIG. 4, the method for producing a mesoporous silica material includes the steps of: (a) mixing H 2 O and EtOH at a constant ratio; (b) adding a surfactant to the solution in which H 2 O and EtOH are mixed at a predetermined ratio; (c) adding a compound selected from the group consisting of a precursor of the mesoporous silica material and a silane functional group to the solution formed in step (b), and stirring the mixture at room temperature for a predetermined time; (d) adding ammonia water to the solution stirred in step (c) and stirring for a predetermined time; (e) washing and drying the material synthesized in the step (d) after filtration; And (f) firing after the step (e).
As described above, the embodiment of the present invention provides a method for producing a mesoporous silica material with a silane-based functional group attached thereto, thereby increasing the specific surface area and improving the adsorption ability according to the structure. The pure mesoporous silica adsorbent It is confirmed that the mesoporous silica adsorbent having a silane-based functional group is excellent in adsorption ability of the mesoporous silica adsorbent, and carbon dioxide is chemically bonded by the functional group on the surface of the mesoporous silica adsorbent, thereby providing a manufacturing method capable of increasing the adsorption amount do.
Further, the steps S100 to S600 except for the firing step (S700) are all performed at room temperature, and the pH is adjusted during the condensation reaction through the addition of the ammonia water of S400. That is, in the synthesis of a conventional mesoporous silica material, a sol is formed by a sol-gel method, and then heat is applied to synthesize a gel. In the embodiment of the present invention, the sol is synthesized at room temperature, It is not a synthesis method, but forms a gel by controlling the pH base. Accordingly, since heat is not applied, it is possible to perform at room temperature, thereby simplifying the process and reducing the cost.
In order to control the pores of the synthesized mesoporous silica material, the concentration ratios of SiO 2 and CTACl were adjusted to 1: 0.1-0.2, and in order to synthesize the mesoporous silica material having a high specific surface area, TEOS The molar concentration is adjusted to 0.1 to 0.4 M to prepare SiO 2 .
The pore structure of the mesoporous silica material can be selected to be a hexagonal structure and a cubic structure by controlling the concentration ratio of SiO 2 and CTACl to 1: 0.1 to 0.2, and preferably, the concentration ratio of SiO 2 to CTACl is 1: When it is set to 0.1 or more and less than 0.15, it can be selected as a hexagonal structure. When the concentration ratio of SiO 2 and CTACl is set to 1: 0.15 or more to 0.2 or less, a cubic structure can be selected. Also, it is possible to increase the specific surface area of the mesoporous silica material by increasing the molar concentration of TEOS in the range of 0.1 to 0.4 M of the TEOS concentration.
Referring to FIG. 4, the process of manufacturing the mesoporous silica material with silane-based functional groups according to an embodiment of the present invention will be described in more detail as follows.
As shown in FIG. 4, synthesis of mesoporous silica material with functional groups is synthesized based on optimum conditions among synthesis of hexagonal mesoporous silica material (HMS) and cubic mesoporous silica (CMS).
As shown in FIG. 4, the process of the synthesis of the mesoporous silica material with functional groups is carried out by first mixing H 2 O and EtOH at a predetermined ratio (S100), and adding CTACl, a surfactant, to the mixed solution (S200) Then, aminosilane, which is a compound selected from the functional group, is added to TEOS, which is a precursor of the mesoporous silica material, and stirred for 10 minutes (S300). 5. Aqueous ammonia was added dropwise a solution (NH 4 OH) was added and (S400), at least about 15 hours, and reacted for one day. (S500) that after the composite material was filtered by washing and drying (S600), sintering (S700) meso Thereby synthesizing a porous silica material.
Results analysis
FIGS. 6 and 7 are graphs showing XRD results of the functional group-attached mesoporous silica material prepared by the manufacturing method according to the embodiment of the present invention. FIG. 6 shows XRD results of a functionalized mesoporous silica material having a hexagonal pore structure, and FIG. 7 is an XRD result of a functionalized mesoporous silica material having a cube pore structure.
Mesoporous silica was synthesized based on mesoporous mesoporous silica (HMS4) and cubic mesoporous silica (CMS3), which had the largest specific surface area among the mesoporous silica materials. 6 and 7 are mesoporous silica bearing an amine group. In the case of FIG. 6, although the uniformity of the pores was lowered due to the functional groups, it was confirmed that the hexagonal mesoporous structure was confirmed by confirming the d (100) peak as the main peak.
Amino groups in the aminosilane used in the synthesis process affect the pH of the solution. As the condensation reaction speeds up, the pores decrease and the specific surface area decreases. In the case of FIG. 7, it was confirmed that the mesoporous silica of the cubic structure was confirmed by confirming the peak of d (211) as the main peak. As shown in Fig. 6, which has a hexagonal structure, the size of the peak is reduced and the uniformity of pores is lowered.
N 2 -sorption was used to measure the specific surface area and pore size and volume of mesoporous silica materials with functional groups. The specific surface area was obtained from the BET relationship using the isothermal adsorption / desorption information of the measured sample, and the pore size and volume were obtained from the BJH relation.
[Table 1] and [Table 2] describe the specific surface area, pore size, and pore volume for mesoporous silica materials with functional groups. It was found that the specific surface area and the pore size were decreased as the amount of silane with functional groups was increased. However, there is a difference in the volume of the pores. This is because the pore size distribution of the BJH method shows a difference in the pore volume because the micropore, that is, pores having a pore size of 2 nm or less is ignored.
Here, Si conc. Represents the Si concentration and BET represents the specific surface area.
As shown in [Table 1] and [Table 2], on the basis of HMS4 and CMS3, the shape and size and distribution of the mesoporous silica with functional groups were analyzed by TEM, and FIGS. 8 and 9 The results are shown in Fig.
Figure 8 is a TEM photograph of a hexagonal mesoporous silica material with amine groups. As shown in FIG. 8, it was difficult to control the pH due to the amine groups at the terminal, which made it difficult to form pores. However, it was found that highly developed pores were uniformly arranged.
9 is a TEM photograph of a cubic mesoporous silica material with amine groups. As shown in FIG. 9, although the size of the pores was slightly reduced due to the functional groups, it was found that the highly uniform pores of the upper, lower, left, and right sides were well developed in the form of cubic structure.
The mesoporous silica samples were analyzed by FT-IR (Fourier transform infrared analyzer) to determine the presence of functional groups such as amine groups and fluorine groups. The results are shown in FIGS. 10 and 11. FIG. 10 is a graph of FT-IR of a mesoporous silica having an amine group attached thereto as a hexagonal pore structure functional group, and FIG. 11 is a graph showing FT-IR results of mesoporous silica having amine groups attached to a cube pore structure Graph.
As shown in FIG. 10 and FIG. 11, it was confirmed that the amine group was present in the synthesized sample by confirming two FT-IR peaks at 2900 to 3000 cm -1 , in which the amine group can be confirmed.
As described above, in the embodiment of the present invention, the structure was controlled by adjusting the concentration ratio of the silica material and the surfactant, and the silica mesoporous material having the largest specific surface area by the structure could be synthesized by adjusting the concentration of the silica material. Based on this, silica mesoporous materials with functional groups were synthesized and their adsorption capacities were evaluated using the synthesized materials as adsorbents.
It was found that the adsorption capacity of the cubic structure was superior to that of the hexagonal structure. This is because the specific surface area of the adsorbent is wider and the adsorption area between carbon dioxide and silica is widened to increase the adsorption amount. It is also found that the mesoporous silica adsorbent having a functional group is more excellent in adsorption ability than the pure mesoporous silica adsorbent. It was found that carbon dioxide was chemically bonded by the functional group on the surface of the mesoporous silica adsorbent and the adsorption amount was increased.
Among the mesoporous silica adsorbents, CMS3 (A2) showed the best adsorption capacity at 4.0588 mol / kg. Compared to the hexagonal structure, the cubic mesoporous silica material has a large specific surface area, which means that the number of functional groups attached to the surface is large. Further, when a large amount of silane material is added to increase the number of functional groups on the surface, The number of functional groups exposed on the surface was reduced, and the adsorption capacity was also decreased.
While the invention has been shown and described with respect to the specific embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. Anyone with it will know easily.
Claims (11)
(a) mixing H 2 O and EtOH at a constant ratio;
(b) adding CTACl to a solution in which the H 2 O and EtOH are mixed at a predetermined ratio;
(c) adding the precursor of the mesoporous silica material and aminosilane to the solution formed in step (b), and stirring the mixture at room temperature for a predetermined time;
(d) adding ammonia water to the solution stirred in step (c) and stirring for not less than 15 hours but not longer than 24 hours;
(e) washing and drying the material synthesized in the step (d) after filtration; And
(f) firing after the step (e);
The concentration ratio of SiO 2 , which is a silica material converted from the precursor of the silica material added in the step (c), and CTACl is 0.1-0.2,
When the concentration ratio of SiO 2 to CTACl is 1: 0.1 or more and less than 0.15, the pore structure of the silica material has a hexagonal structure,
Wherein the pore structure of the silica material has a cubic structure when the concentration ratio of SiO 2 to CTACl is 0.15 or more to 0.2 or less.
Wherein the step (c) comprises adding TEOS as the precursor to the mesoporous silica material.
Wherein the molar concentration of the TEOS is in the range of 0.1 to 0.4 M and the molar concentration is increased to increase the specific surface area of the silica material within the range.
Wherein the pH of the solution is set in a range of 9 to 11 by adding ammonia water in the step (d).
Wherein the steps (a) to (e) are performed at room temperature.
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| PCT/KR2015/002044 WO2015199313A1 (en) | 2014-06-26 | 2015-03-03 | Method for preparing mesoporous silica material having silane-based functional group attached thereon |
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