TWI675734B - Manufacturing apparatus of plate type aerogel composites, substrate supporting apparatus for manufacturing plate type aerogel composites and manufacturing method of plate type aerogel composites - Google Patents

Abstract

The invention provides a plate-shaped aerogel composition preparation device and a plate-shaped aerogel. Substrate support device for preparing glue composition and method for preparing plate-shaped aerogel composition. The device for preparing plate-shaped aerogel composition includes a substrate support device, which divides a space by a separation part, and divides and stores the space. 2 or more substrates; a chamber that houses a substrate support device; and a solution supply section that supplies a sol solution or a cleaning solution to the substrate storage section; according to the above method and device, it is relatively simple and efficient to standardize the size A plate-like aerogel composition having a good surface was prepared.

Description

Plate-shaped aerogel composition preparation device, plate-shaped aerogel composition Substrate support device for product preparation and method for preparing plate-shaped aerogel composition

The invention relates to a device for preparing a plate-like aerogel composition and a method for preparing a plate-like aerogel composition using the same.

The aerogel discovered by Kistler in the early 1930s, as a dry gel with high porosity, is known as the substance with the lowest thermal conductivity at present. Generally, aerogels have a high porosity of more than 90% and a maximum of about 99%. Among the materials developed by humans so far, they have the most excellent ultra-insulation / ultra-porosity / ultra-lightweight / ultra-low dielectric Electrical constants and other characteristics, therefore, it is a promising material with unlimited application potential in various fields such as energy-saving materials, sound-absorbing materials, and fire-resistant materials in the fields of buildings, industries, aerospace, and shipbuilding. Aerogels are classified into felts (composition, Blank, flakes), powders, and monoliths according to their morphology.

Aerogels can be prepared by the following methods: After a sol-gel polymerization reaction is performed on the silica precursor solution to make a wet gel, the supergel is under supercritical or atmospheric conditions. Dry. Considering the low workability of powder aerogels, aerogels in the form of felts are used. Such aerogels in the form of felts are mostly prepared by a continuous process using a roll-to-roll form.

[Prior technical literature]

[Patent Literature]

Korean Patent Laid-Open Publication No. 10-2006-0025564, a method for manufacturing a gel sheet

Korean Patent Publication Gazette No. 10-2012-0028635, Manufacturing method of silica aerogel composite plate

An object of the present invention is to provide a plate-shaped aerogel composition preparation device for preparing a plate-shaped aerogel composition with a good surface according to a standardized size, and a method for preparing a plate-shaped aerogel composition using the same.

In order to achieve the above-mentioned object, an apparatus for preparing a plate-like aerogel composition according to an embodiment of the present invention includes: i) a substrate supporting apparatus (substrate supporting apparatus), which divides and separates two or more spaces in space by dividing a space by a separation unit; The substrate includes a first substrate accommodating portion, a second substrate accommodating portion, and a separation portion. The first substrate accommodating portion is a space that accommodates the first substrate and has a length in the x direction and a length in the y direction. And the z-direction length plate type, the z-direction length value is greater than the x-direction length value or the y-direction length value, and the second substrate receiving portion is a space that is adjacent to the first substrate receiving portion and It is spatially distinguished from the first substrate containing portion and The second substrate is accommodated, and the separation portion is located between the first substrate accommodation portion and the second substrate accommodation portion to distinguish two spaces, including the substrate accommodation of the first substrate accommodation portion and the second substrate accommodation portion. The lower or upper end of the unit is open; ii) a chamber that houses the substrate support device inside; and iii) a solution supplying part that supplies a sol solution or a cleaning solution to the substrate receiving unit (washing solution).

The separation portion may have a wall shape, and an upper end and a lower end of the substrate receiving portion are open.

The separation portion may have a columnar shape including a front surface, a left surface, a back surface, and a right surface. The substrate receiving portion is a space surrounded by the above-mentioned column-shaped separation portion, and the upper and lower ends thereof are open.

The separation portion may be a barrier type, and blocks fluid from moving between the first substrate receiving portion and the second substrate receiving portion in the x direction or the y direction.

The separation portion may be a mesh type or have multiple openings (holes, pores), allowing the fluid to move in the x direction or the y direction between the first substrate receiving portion and the second substrate receiving portion.

The plate-shaped aerogel composition preparation device may further include a decompression device that decompresses the substrate storage portion.

The plate-shaped aerogel composition preparation device may further include a lower end support portion located at a lower end of the substrate support device and supporting the substrate support device.

The lower end support portion allows the fluid to move in the z direction between one surface of the lower end support portion and the lower end of the substrate receiving portion.

The substrate receiving portion may have an open upper end.

The plate-shaped aerogel composition preparation device can be further modified on the upper part of the substrate supporting device. Including the upper end fixing portion.

The upper-end fixing portion may further include a fluid storage portion that accommodates the sol solution or the cleaning solution supplied from the solution supply portion and moves the sol solution or the cleaning solution to the substrate storage portion.

The plate-shaped aerogel composition preparation device may further include a solution storage unit that recovers the sol solution or the cleaning solution supplied to the substrate supporting device.

The substrate supporting device for preparing a plate-like aerogel composition according to another embodiment of the present invention divides a space by a separation section, and divides and stores two or more substrates in space, and includes: a first substrate accommodating section Is a space that houses the first substrate in a plate type having an x-direction length, a y-direction length, and a z-direction length, and the z-direction length value is greater than the x-direction length value or the y-direction length value; The second substrate receiving portion is a space adjacent to the first substrate receiving portion, spatially distinguishing from the first substrate receiving portion and accommodating the second substrate; and a separating portion located on the first substrate. Two spaces are distinguished between the accommodating portion and the second substrate accommodating portion; and the lower end or the upper end of the substrate accommodating portion including the first substrate accommodating portion and the second substrate accommodating portion is open.

The separation portion may have a wall shape, and an upper end and a lower end of the substrate receiving portion are open.

The separation portion may have a columnar shape including a front surface, a left surface, a back surface, and a right surface. The base material receiving portion is a space surrounded by the column-shaped separation portion, and the upper and lower ends thereof are open.

The separation portion may be a barrier type, and blocks fluid from moving between the first substrate receiving portion and the second substrate receiving portion in the x direction or the y direction.

The separation portion may be a mesh type or have a plurality of holes (pores, pores), allowing the fluid to move between the first substrate receiving portion and the second substrate receiving portion in the x direction or the y direction.

The substrate supporting device may further include a lower end portion, which is located at the lower end of the substrate supporting device and supports the substrate received in the substrate receiving portion, and allows the fluid to move in the z direction.

The substrate receiving portion may have an open upper end.

The substrate supporting device may further include an upper end portion, which is located above the open upper end, and allows the fluid to move in the z direction.

A method for preparing a plate-shaped aerogel composition according to another embodiment of the present invention includes an impregnation step of supplying a sol solution to a substrate supporting device, and preparing a plate-shaped substrate located in a substrate receiving portion and impregnated with the sol solution, That is, the substrate is impregnated. The substrate supporting device includes two or more substrate storage sections and separation sections, and a plate-shaped substrate is stored in the substrate storage section. The two or more substrate storage sections are as follows. A plate type having an x-direction length, a y-direction length, and a z-direction length. The z-direction length value is greater than the x-direction length value or the y-direction length value. The separation section spatially distinguishes the above-mentioned substrate storage sections adjacent to each other. ; An aging step to induce gelation and aging of the sol solution contained in the impregnated substrate to prepare a gelled substrate; a device removal step to self-gelate the substrate through the open upper or lower end of the substrate containing portion Separating the substrate supporting device; and a solvent removing step, removing the solvent from the gelled substrate to prepare an aerogel composition.

The aging step can be performed in a state where the pressure in the substrate accommodating section or the substrate supporting device is reduced to 300 Torr or less by a pressure reducing device.

When the substrate storage portion uses the smaller of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a value that is five times or more the above-mentioned reference value.

The solvent removal step may further include a washing process. The cleaning process can be performed in sequence of 1 cleaning, 2 cleanings and 3 cleanings. The 1st cleaning application includes 1st cleaning solution of distilled water, the 2nd cleaning application includes 2nd cleaning solution of acetone, and the 3th cleaning application includes selection. 3-times cleaning solution of alcohol in a group consisting of propanol, butanol, and combinations thereof.

The solvent removal step may further include a recombination process. The recombination process can be performed by applying a recombination solution including an organic solvent and a silane compound in a weight ratio of 1: 0.1 to 1: 1 to a gelled substrate or a gelled substrate after a cleaning process.

The solvent removal step is a process of removing the solvent from the gelled substrate, and can be applied to the gelled substrate, the gelled substrate after the cleaning process, or the gelled substrate after the recombination step. The solvent removal step can be performed by normal pressure drying, supercritical drying, or alternately by normal pressure drying and supercritical drying.

In the case of applying atmospheric drying in the solvent removal step, it can be performed by: cleaning the gelled substrate with hexane, the gelled substrate after the cleaning process, or the gelled substrate after the recombination step. After the material is left, it is left in an air environment at 5 ° C to 350 ° C for 60 minutes to 600 minutes.

The substrate inserted into the substrate receiving portion in the impregnation step may be one that satisfies the following conditions: the smaller of the x-direction length and the y-direction length of the substrate is the reference value, and the x-direction of the corresponding substrate receiving portion The smaller value between the length and the y-direction length is 1.05 to 3.00 times the above-mentioned reference value.

A method for preparing a plate-shaped aerogel composition according to another embodiment of the present invention includes an impregnation step of accommodating a plate-shaped substrate on a plate-shaped lower end portion of a substrate-supporting device that has fluid permeability, so as to have a fluid. The permeable upper end portion fixes the upper end of the substrate support device and supplies a sol solution to prepare a plate-shaped substrate, ie, an impregnated substrate, which is located in the substrate storage portion and is impregnated with the sol solution. The substrate support device includes two or more substrates. Material storage section and fluid-permeable separation section, and the two or more substrate storage sections are spaces that have a plate type having a length in the x direction, a length in the y direction, and a length in the z direction, and a length in the z direction Value is greater than the length in the x direction or the length in the y direction Value, the fluid-permeable separation section spatially distinguishes adjacent substrate storage sections; the aging step induces gelation and aging of the sol solution contained in the impregnated substrate to prepare a gelled substrate; the device moves Step of moving the substrate supporting device to a solvent removing device, the substrate supporting device comprising a gelled substrate located in the substrate containing portion, and including a separation portion, an upper end portion and a lower end portion combined with each other; and a solvent removing step, in In the solvent removing device, the solvent is removed from the gelled substrate to prepare an aerogel composition.

The aging step can be performed in a state where the pressure in the substrate accommodating part or the substrate supporting device is reduced to 300 Torr or less by a pressure reducing device.

When a smaller value of the length value in the x-direction or the length value in the y-direction is used as the reference value, the length value in the z-direction may have a value that is five times or more the reference value.

The solvent removal step may further include a cleaning process. The cleaning is performed in sequence of 1 cleaning, 2 cleanings, and 3 cleanings. 1 cleaning application includes 1 cleaning solution of distilled water, 2 cleaning applications includes 2 cleaning solutions of acetone, 3 Secondary cleaning applications include three cleaning solutions of alcohols selected from the group consisting of propanol, butanol, and combinations thereof.

The solvent removal step may further include a recombination process. The recombination is performed by applying a recombination solution including an organic solvent and a silane compound in a weight ratio of 1: 0.1 to 1: 1 to the above-mentioned gelled substrate or undergoing the above-mentioned cleaning process. Gelled substrate.

The solvent removal step is a process of removing the solvent from the gelled substrate, and can be applied to the gelled substrate, the gelled substrate after the cleaning process, or the gelled substrate after the recombination step. The solvent removal step can be performed by normal pressure drying, supercritical drying, or alternately by normal pressure drying and supercritical drying.

In the case of applying atmospheric drying in the solvent removal step, it can be performed by: cleaning the gelled substrate with hexane, the gelled substrate after the cleaning process, or the gelled substrate after the recombination step. After the material, an air ring at 5 ° C to 350 ° C Leave in the environment for 60 minutes to 600 minutes.

The substrate inserted into the substrate receiving portion in the impregnation step may be one that satisfies the following conditions: the smaller of the x-direction length and the y-direction length of the substrate is the reference value, and the x-direction of the corresponding substrate receiving portion The smaller value between the length and the y-direction length is 1.00 times to 3.00 times the above-mentioned reference value.

The plate-shaped aerogel composition preparation device of the present invention and the method for preparing a plate-shaped aerogel composition using the same can prepare plate-shaped aerogel compositions with a good surface in a standardized size, and the preparation steps thereof are also relatively simple and feasible. Efficiently provide a plate-like aerogel composition with a good surface.

10‧‧‧ Substrate

20‧‧‧ Substrate storage section

30‧‧‧ Separation Department

33‧‧‧ Front

34‧‧‧Back

100‧‧‧ substrate support device

200‧‧‧ chamber

300‧‧‧ Solution Supply Department

310, 610, 710‧‧‧ Control Valve

400‧‧‧ lower support

500‧‧‧ Upper fixed part

600‧‧‧ Decompression device

700‧‧‧Solution Recovery Department

900‧‧‧ plate-shaped aerogel composition preparation device

1 (a) and 1 (b) are conceptual views of a plate-like substrate storage portion described in the present invention.

FIG. 2 is a conceptual diagram illustrating a plate-shaped aerogel composition preparing device according to an embodiment of the present invention.

FIG. 3 is a conceptual diagram showing a structure of a substrate supporting device according to an embodiment of the present invention.

FIG. 4 (a) is a cross-sectional view when the separation section in FIG. 3 is in the form of a column, and FIG. 4 (b) is a cross-sectional view when the separation section is in the form of a column.

5 (a) is a cross-sectional view showing a state where a base material is stored in a base material supporting device according to an embodiment of the present invention, and FIG. 5 (b) is a cross-sectional view showing a state where the base material supporting device is separated from the base material.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings, so that those skilled in the art to which the present invention pertains can easily implement them.

However, the present invention can be implemented in various forms, and is not limited to the embodiments described herein. Throughout the description, similar parts are marked with the same symbols.

Throughout the description, terms such as "first", "second" or "A" and "B" are used to distinguish the same terms.

Throughout the description, B located on A means that B is located on A, or other layers may be positioned therebetween so that B is located on A, and is not limited to interpreting B as positioned in contact with the surface of A.

Throughout the description, the term "combination" included in the expression of the Markush form means a mixture or combination of one or more selected from the group consisting of the constituent elements described in the expression of the Markush form, meaning The author includes one or more members selected from the group consisting of the aforementioned constituent elements.

Throughout the description, unless otherwise specified, expressions in the singular number are construed to include the singular or plural number according to the context.

Throughout the description, "steps to perform ~" or "steps to ~" do not mean "steps to ~".

1 (a) and 1 (b) are conceptual diagrams illustrating a plate-like substrate storage portion of the present invention, and FIG. 2 is a conceptual diagram illustrating a plate-like aerogel composition preparing apparatus according to an embodiment of the present invention. FIG. 3 is a conceptual view showing a structure of a substrate supporting device according to an embodiment of the present invention, and FIG. 4 (a) is a cross-sectional view when the separation portion in FIG. 3 is in the form of a column when viewed along the direction aa ', Fig. 4 (b) shows the case where the separation part is in the form of a column. 5 (a) and 5 (b) are cross-sectional views showing a state where a substrate is stored in a substrate supporting device according to an embodiment of the present invention, and FIG. 5 (a) shows the substrate is stored in a substrate FIG. 5 (b) shows the state of the substrate accommodating part of the material supporting device, and the state where the substrate is separated from the substrate supporting device. Hereinafter, the present invention will be described with reference to FIGS. 1 (a) to 5 (b).

An apparatus for preparing a plate-like aerogel composition according to an embodiment of the present invention includes: i) a substrate supporting apparatus 100 (substrate supporting apparatus), which divides a space by a separation unit 30 and distinguishes two or more substrates in space; 10 to be accommodated in the substrate accommodating section 20; ii) a chamber 200 (chamber) to house the substrate supporting device 100 therein; and iii) a solution supplying part 300 (solution supplying part) to supply to the substrate accommodating section 20 Sol solution or cleaning solution.

The substrate accommodating section 20 is a space for accommodating the substrate 10 during the process of preparing the plate-shaped aerogel composition. Two or more substrate accommodating sections 20 are disposed in the substrate supporting device 100.

The substrate accommodating portion 20 is a plate type space having a length in the x direction, a length in the y direction, and a length in the z direction, and is characterized in that the length value in the z direction is greater than the length value in the x direction or the length value in the y direction (see FIG. 1 ( a) and Figure 1 (b)).

According to the context, the substrate storage section 20 includes a first substrate storage section 20 and a second substrate storage section 20. As described above, in order to distinguish the plurality of substrate storage sections 20 from each other, such as "first", " "Second" is used to explain.

The substrate supporting device 100 includes: a first substrate accommodating portion 20 that accommodates the first substrate 10; and a second substrate accommodating portion 20 that is a space adjacent to the first substrate accommodating portion 20, Is spatially distinguished from the first substrate storage portion 20 and accommodates the second substrate 10; and a separation portion 30 is located at the first substrate storage portion 20 Two spaces are distinguished from the second substrate storage portion 20 described above.

The separation section 30 spatially distinguishes two adjacent substrate storage sections 20 and supports the substrate 10 stored in the substrate storage section 20 described above. Even if a fluid flow occurs during the application of the preparation method, the substrate 10 Deformation or movement is restricted within the substrate storage portion 20.

In addition, since the impregnation and gelation of the substrate 10 described below is performed in the substrate accommodating section 20, the aerogel composition prepared in such a substrate accommodating section 20 has the advantage of being in a standardized form even if The separation membrane, which is mainly used in the roll-to-roll process, has good characteristics such as flat surface and relatively constant aerogel density.

The substrate storage portion 20 is a plate-type space whose length in the z direction is greater than the length in the x direction or the length in the y direction. Therefore, the entire shape of the substrate 10 stored in the substrate storage portion is also the same as the substrate storage It is in the form of a plate, and at the same time, the surface (xy plane) with a smaller area equivalent to the thickness of the plate is located at the lower end of the substrate storage portion, that is, "the state of standing by the thickness (the state of standing by the thickness) ) "Containment. Therefore, if there is no other support unit such as the separation unit 30, it is difficult to maintain the "standing state with a thickness" especially in the internal environment of the substrate support device where fluid flow (including the flow of solution or air) occurs, but In the present invention, the separation portions 30 located on both sides of the substrate accommodation portion 20 are supported so that the substrate 10 can be stably stood on a smaller surface corresponding to the xy surface.

The z-direction length value of the substrate storage portion 20 is greater than the x-direction length value or the y-direction length value, and thus the substrate storage portion constituting the z-direction length value is smaller than the x-direction length value or the y-direction length value of the substrate storage portion, respectively. Compared to the situation, there are several advantages.

First of all, the substrate storage portion 20 of the present invention has the advantage that it is advantageous to form an aerogel richly on two x-z planes and two y-z planes with a wide area. Nanopores formed during the gelation process during the preparation of the aerogel composition not only need to be well formed, but must not collapse during the preparation process such as cleaning or recombination. The nano-pores on the x-y plane formed at the lowermost end of the substrate are prone to collapse due to fluid movement or load on the substrate during the above-mentioned preparation process. The substrate accommodating part 20 of the present invention minimizes the area of the lowermost end surface (xy plane) of the substrate 10 itself, minimizes the possibility of collapsing the nanopores, and maximizes the area of the other surfaces, thereby making it possible to It is easy to prepare an aerogel composition having an excellent pore structure as a whole.

In addition, the substrate containing portion 20 of the present invention has a narrower xy plane at the lowermost end surface, and therefore constitutes a substrate whose length value in the z direction is smaller than the length value in the x direction and the length in the y direction of the substrate containing portion. Compared with the case of the accommodating part, there is also an advantage that the phenomenon that the base material can be prevented from sagging. If the process of impregnation and cleaning is performed in accordance with the "transverse state with a wider surface", a drooping phenomenon of the central portion of the wider surface sinking in the direction of gravity will occur. A stand is additionally provided. However, the provision of such a bracket complicates the structure of the substrate supporting device, and in particular, in the process of inserting or removing the substrate into the substrate accommodating portion, the workability is reduced, which may cause the efficiency of the manufacturing process to be reduced. one.

In the present invention, the length of the z-direction length of the substrate accommodating portion 20 is larger than the length of the x-direction or the length of the y-direction. Therefore, even if a separate membrane is not applied, the nanopores of the entire substrate 10 collapse. The problem is also minimized, and an aerogel composition having an excellent pore structure, a flat surface, and a fixed surface property can be prepared.

Specifically, when the substrate storage portion 20 uses a smaller value of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a reference value of 5 Multiples. More specifically, when the substrate storage portion 20 uses the smaller of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a value that is 10 times or more the reference value. More specifically, when the substrate storage portion 20 uses the smaller of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a value of 50 to 300 times the reference value. When a substrate containing portion having such a length value is applied, an aerogel composition having more excellent characteristics can be prepared over a wide area.

When the smaller value of the x-direction length value and the y-direction length value of the substrate 10 inserted into the substrate storage portion 20 is the "base material reference value", the x direction of the substrate storage portion 20 corresponding thereto The smaller of the length value and the length value in the y direction, that is, the "length value of the substrate receiving portion" may be 1.00 times to 3.00 times the reference value of the above substrate, specifically 1.05 times to 2.5 times, and more specifically It can be 1.05 times to 2.0 times. When the substrate storage portion 20 is compared with the reference value of the substrate described above and the length of the corresponding substrate storage portion is 3.00 times or more, the substrate 10 cannot be sufficiently supported by the substrate storage portion 20 In the case of less than 1.00 times, the impregnation of the sol solution may be insufficient. In addition, when the substrate storage portion 20 is compared with the reference value of the substrate described above and the corresponding length value is 1.05 to 2.0 times, it is advantageous to prepare an aerogel composition with a flat surface and a fixed surface property. Thing.

In this case, the length in the z direction may be any length as long as the length in the z direction of the substrate storage portion is longer than the length in the z direction of the substrate 10. In addition, as for the larger value of the length in the x direction and the length in the y direction, the corresponding length of the substrate accommodating portion may be longer than the corresponding length of the substrate 10.

The substrate supporting device 100 may include two or more, that is, a plurality of substrate accommodating portions 20. In this case, a plate-shaped aerogel composition having a relatively uniform quality can be prepared in a manner of being produced in large quantities at the same time.

The plurality of substrate accommodating portions 20 can be formed by forming a plurality of wall shape separation portions 30 in the substrate supporting device 100 at regular intervals. In the case where the separation portion 30 having a wall shape is formed as described above, there is an advantage that it is easier to adjust the width (the length in the x direction or the length in the y direction) of the substrate storage portion 20.

The plurality of substrate accommodating portions 20 can be formed by arranging columnar shape separation portions 30 side by side in the substrate supporting device 100. The separation part 30 in the above-mentioned pillar form has a form including a front face, a left side face, a back face, and a right side face, and the substrate accommodating part 20 is located inside the pillar. In the case of forming the separation portion 30 in such a column shape, there is an advantage that the base material storage portion 20 can be formed more firmly.

The substrate supporting device 100 including the separation portion 30 in the above wall form can position the front portion 33 and the back portion 34 on the front and back sides substantially at right angles to the length direction of the separation portion 30, respectively. Wall shape. The front surface portion 33 and the rear surface portion 34 play a role of restricting the movement of the substrate to the front and back surfaces of the substrate storage portion 20 located in the substrate support device 100.

Specifically, the front part 33 may further include a receiving groove (not shown) for receiving one end of the separation part 30, and the rear part 34 may further include a receiving groove (not shown) for receiving the other end of the separation part 30. As described above, when the separation portion 30 is fixed by the front portion 33, the back portion 34, or the accommodation grooves formed in the front portion and the back portion, the position of the separation portion 30 can be held more firmly.

In addition, the separation portion 30 can be fixed by coupling the housings (not shown) of the substrate supporting device with the upper and lower ends open.

The substrate accommodating portion 20 may be an open end or a lower end, and may be an open end of both the upper end and the lower end.

When the upper end of the substrate accommodating section 20 is open, the open upper The base material 10 can be easily inserted. In addition, when the upper end of the substrate storage portion 20 is open, the sol solution or the cleaning solution can be easily poured into the substrate storage portion by the opened upper end.

When the lower end of the substrate storage section 20 is open, the separation section 30 or the substrate support device 100 can be separated from the substrate 10 located in the substrate storage section 20 and easily removed.

Specifically, the separation unit 30 or the substrate supporting device 100 can make the substrate 10 be located in the chamber 200 in the original state by a relatively simple process of lifting upward in a state where the substrate 10 is located in the substrate receiving portion 20. The separation portion 30 between the first base material 10 and the second base material adjacent to each other is easily removed (see FIG. 5 (b)).

At this time, the substrate 10 may be (a) an impregnated substrate that has undergone an impregnation process, a gelled substrate that is being gelled or has been gelled, or (b) that has undergone an impregnation process. Wash and reconstitute aerogel composition. As described above, in the case where the substrate of the aerogel composition is being prepared instead of the substrate that was initially inserted, as the preparation process progresses, the substrate is subjected to gelation of the sol solution to have a narrow xy area. The surface is located at the lowermost end, so that even if the z-direction length value is greater than the x-direction length value or the y-direction length value, the "stand-up state with thickness" can be stably maintained inside the chamber 200. Thereafter, the required process can be simply performed An aerogel composition having excellent quality is prepared.

The substrate supporting device 100 may further include a coupling unit (not shown) that connects and separates the plurality of separation portions 30 in the form of walls.

The substrate supporting device 100 may include a coupling unit (not shown) that fixes the front portion 33 and the rear portion 34 together with the plurality of separation portions 30 in the form of walls.

The substrate supporting device 100 may further include a separation section 30 for separating a plurality of columns. This connection and fixing unit (not shown).

The separation part 30 may be a barrier type and has fluid impermeability. Specifically, the partition-like separation portion 30 can block fluid from moving between the first substrate receiving portion and the second substrate receiving portion in the x direction or the y direction. As a material of the partition wall, a material having chemical resistance can be applied, and specifically, stainless steel, a coated metal, glass, or a combination thereof can be applied.

The separation part 30 may be a mesh type, have a mesh shape as a whole, or have a plurality of openings (holes, pores), and have fluid permeability. Specifically, the mesh-shaped separation portion 30 may allow the fluid to move in the x direction or the y direction between the first substrate receiving portion and the second substrate receiving portion through a mesh or an opening.

As the material of the mesh-like or separated portion having a plurality of openings, a material having chemical resistance can be applied. Specifically, a stainless steel mesh, a coated metal mesh, a fluid-permeable glass fiber, and a corrosion-resistant polymer can be applied. Tablets or combinations thereof.

The substrate supporting device 100 may further include a lower end portion (not shown). The substrate supporting device 100 is located at the open lower end of the substrate supporting device and supports the substrate 10 accommodated in the substrate receiving portion 20 to allow the fluid to move in the z direction.

The substrate supporting device 100 may further include an upper end portion (not shown), which is located at the open upper end of the substrate accommodating portion and allows the fluid to move in the z direction.

As the material of the lower end portion or the upper end portion, a material having chemical resistance can be applied, and specifically, a stainless steel mesh, a coated metal mesh, a fluid-permeable glass fiber, a corrosion-resistant polymer sheet, or a combination thereof can be applied.

The plate-shaped aerogel composition preparing device 900 may further include a pressure reducing device 600 for reducing the pressure of the substrate containing portion 20.

The substrate storage section 20 using the pressure reducing device 600 can be performed as follows. Decompression performed: Only the substrate accommodating portion 20 is decompressed; the substrate supporting device 100 including the substrate accommodating portion 20 is decompressed; or the entire interior of the chamber 200 including the substrate supporting device 100 is maintained as Decompression state.

Specifically, the decompression device 600 may be connected to the chamber 200 or the substrate support device 100 to decompress the substrate accommodating portion 20. The connection may be directly connected to the chamber 200, directly connected to the substrate support device 100, It is connected to the lower end support part 400 located below the base material supporting device 100 and to the upper end fixing part 500 located on the base material supporting device 100.

The pressure reducing device 600 may be connected to a control valve 610 that controls the degree of pressure reduction.

Maintaining the reduced pressure can help to quickly and sufficiently supply the sol solution or the cleaning solution to the substrate accommodating portion 20 and penetrate into the substrate 10, and effectively remove the surface tension caused by the fibers in the substrate. bubble.

The decompression state can be a decompression state of 300 Torr or less based on the absolute pressure inside the substrate accommodating section 20, the substrate support device 100, or the chamber 200, and can be a decompression state of 0.001 Torr to 300 Torr, 0.001 Torr to 100 Torr decompression state or 0.001 Torr to 10 Torr decompression state.

The plate-shaped aerogel composition preparation device 900 may further include a lower end support portion 400 located at the lower end of the substrate support device 100 and supporting the substrate support device 100.

The lower end support portion 400 may be disposed integrally with the cavity 200 or separately. The lower end support portion 400 may be in a flat plate form or a flat plate form having a receiving groove (not shown) for receiving the substrate supporting device 100.

The lower end support part 400 allows fluid to move in the z direction between one surface of the lower end support part 400 and the lower end of the base material storage part 20. Specifically, the lower end support part 400 itself may be a mesh type or have a plurality of holes. In addition, The lower end support portion 400 can be positioned at the lower end of the substrate receiving portion 20 to a surface on the lower end support portion 400 with a slit, a net, or a plurality of openings.

The lower support portion 400 may further include a fluid storage portion (not shown) that can move or store a fluid therein. The fluid storage portion is connected to the solution supply portion 300 through a solution inflow portion (not shown), so that the fluid can be removed from the solution. The supply unit receives and receives the sol solution or the cleaning solution. The sol solution or the cleaning solution contained in the fluid containing section can be introduced into the substrate contained in the substrate containing section 20 by the pressure supplied from the solution supply section, the decompression of the substrate containing section 20, or the pressure and decompression. 10.

The lower support portion 400 may further include a fluid containing portion (not shown) that can move or contain a fluid inside. The fluid containing portion is controlled by the pressure reducing device 600, and can be used for the fluid containing portion (not shown) and a substrate connected thereto. The density of the air, that is, the air pressure, of the accommodation section 20 is adjusted. Specifically, if the fluid storage section is decompressed by the pressure reducing device, the base storage section 20 connected to the lower end support section 400 and allowing the fluid to move in the z direction may be decompressed. When the pressure is reduced as described above, bubbles generated between the fibers of the substrate can be minimized.

The substrate storage portion 20 has an open upper end. The plate-shaped aerogel composition preparation device 900 may further include an upper end fixing portion 500 on the upper portion of the substrate support device 100.

The upper end fixing portion 500 may be in the form of a flat plate or in the form of a flat plate having a receiving groove (not shown) for receiving the substrate supporting device 100.

The upper end fixing portion 500 may be fixed and released from the substrate supporting device 100. When the upper fixing portion 500 is decoupled from the substrate supporting device 100, the upper fixing portion 500 may be removed from the substrate supporting device 100 and positioned separately. .

The lower end of the upper end fixing portion 500 may allow the fluid to move in the z direction between the fluid and the upper end of the substrate containing portion 20. Specifically, at least one of the upper end fixing portions 500 The face itself may be a mesh type as a whole or have multiple holes. In addition, at least one side of the upper end fixing portion 500 may have a slit, a net, or a plurality of openings at a position of the upper end fixing portion 500 corresponding to the upper end of the substrate containing portion 20. In this case, even if the upper end fixing portion 500 is provided, the fluid can move toward the upper end of the substrate containing portion 20 in the z direction. Specifically, the solution or air can move.

The upper end fixing portion 500 may further include a fluid storage portion (not shown) that stores fluid inside and moves the fluid toward the base material storage portion 20, and the fluid storage portion is connected to the solution supply portion 300 through a solution inflow portion (not shown). They are connected to each other, and can receive and receive a sol solution or a cleaning solution from the solution supply unit. The sol solution or the cleaning solution contained in the fluid containing section can be introduced into the substrate contained in the substrate containing section 20 by the pressure supplied from the solution supply section, the decompression of the substrate containing section 20, or the pressure and pressure. 10.

The upper fixed part 500 may further include a fluid storage part (not shown) that moves or stores fluid inside. The fluid storage part is controlled by the pressure reducing device 600 and can hold the fluid storage part (not shown) and a substrate connected thereto. The air density of the section 20, that is, the air pressure is adjusted. Specifically, if the fluid storage portion is decompressed by the pressure reduction device, the base material storage portion 20 connected to the upper end fixing portion 500 to allow the fluid to move in the z direction may be decompressed. When the pressure is reduced as described above, bubbles generated between the fibers of the substrate can be minimized.

The upper end fixing portion 500 functions as a coupling unit of the separation portion 30 that is coupled to the plurality of separation portions 30 and fixes the separation portions to each other. As described above, when the upper-end fixing portion 500 functions to couple and fix the plurality of separation portions 30 to each other, the method of removing the upper-end fixing portion 500 from the chamber in a state where the separation portions 30 are fixed can be simply performed. The substrate supporting device 100 is separated from the substrate 10.

The plate-shaped aerogel composition preparation device 900 may further include a solution recovery unit 700 that recovers the sol solution or the cleaning solution supplied to the substrate support device 100 or the substrate storage portion 20.

The solution recovery part 700 may be connected to the chamber 200.

The solution recovery part 700 may be connected to the lower end support part 400.

The solution recovery part 700 may be connected to the substrate supporting device 100.

The solution recovery part 700 may be connected to the upper end fixing part 500.

The solution recovery unit 700 may be connected to a control valve 710 that controls a solution flowing into the solution recovery unit 700.

The sol solution or the cleaning solution recovered by the solution recovery unit 700 can be moved to a solution supply unit that supplies the sol solution or a solution supply unit that supplies the cleaning solution, respectively. In order to realize the above-mentioned movement, it can be applied to a process used in a general solution reuse process. Specifically, a filter (not shown) for removing foreign matter from the recovered solution, and a pump (not shown) for moving the solution can be applied. (Shown), and a control valve 710 that controls movement.

The chamber 200 plays a role of accommodating the substrate supporting device 100 therein, and seals the inside of the chamber when a sol solution or a cleaning solution is supplied, or when the substrate accommodating portion 20 is decompressed. In addition, the upper or lower end of the chamber 200 may be opened, and the substrate supporting device 100 or the substrate 10 may be smoothly moved by the opened upper or lower end.

The solution supply unit 300 may supply a sol solution to the substrate 10 or the substrate storage unit 20.

The solution supply unit 300 may be connected to the chamber 200 or the substrate support device 100 directly or through other components, and the sol solution is supplied through the control valve 310. In a state of being connected to the chamber 200, the sol solution can be supplied to the substrate supporting device 100, the substrate storage portion 20, or the substrate 10.

The above connection may be directly connected to the chamber 200, directly connected to the substrate support device 100, connected to the lower end support portion 400 located below the substrate support device 100, and connected to the upper end fixed portion 500 located on the substrate support device 100. .

The solution supply part 300 can supply a cleaning solution to the substrate storage part 20 or the substrate 10.

The solution supply unit 300 is connected to the chamber 200 or the substrate support device 100 directly or through other components, and the cleaning solution is supplied through the control valve 310. The substrate supply device can be connected to the substrate support device without being directly connected to the chamber 200. 100. The substrate 10 located in the substrate storage portion 20 or the substrate 10 in a state where the separation portion 30 is removed is supplied with a cleaning solution.

The above connection may be directly connected to the chamber 200, directly connected to the substrate support device 100, connected to the lower end support portion 400 located below the substrate support device 100, and connected to the upper end fixed portion 500 located on the substrate support device 100. .

The solution supply unit 300 may be connected to a control valve 310 that controls a solution supplied by the solution supply unit 300.

When the plate-shaped aerogel composition preparation device 900 is applied for the purpose of impregnation and gelation, the solution supply unit 300 may be used to supply a sol solution.

When a plate-shaped aerogel composition preparation device 900 is applied for the purpose of cleaning and reorganization, the solution supply unit 300 can be used to supply a cleaning solution. In addition to the cleaning solution, a reconstituted solution may be further included. The cleaning solution and the reconstituted solution may be stored in separate spaces, and immediately after the solution is supplied by stirring by a stirring unit, the cleaning solution and the reconstituted solution may be sequentially supplied.

The substrate supporting device 100 for preparing a plate-like aerogel composition according to another embodiment of the present invention divides a space by a separation section 30, and divides and accommodates two or more substrates in space. The substrate includes: a first substrate The material accommodating portion 20 is a space for accommodating the first substrate 10 in a plate shape having an x-direction length, a y-direction length, and a z-direction length, and the z-direction length value is greater than the x-direction length value or the y-direction length value; The second substrate storage portion 20 is a space adjacent to the first substrate storage portion 20 and is spatially distinguished from the first substrate storage portion 20 and accommodates the second substrate 10; and the separation portion 30 is located at the first A substrate receiving portion 20 and a second substrate receiving portion 20 define two spaces; and the lower or upper ends of the substrate receiving portion 20 including the first substrate receiving portion 20 and the second substrate receiving portion 20 are open. .

Specifically, when the substrate storage portion 20 uses the smaller of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a value that is five times or more the reference value. More specifically, when the substrate storage portion 20 uses the smaller of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a value that is 10 times or more the reference value. More specifically, when the substrate storage portion 20 uses the smaller of the x-direction length value or the y-direction length value as a reference value, the z-direction length value may have a value of 50 to 300 times the reference value. When a substrate containing portion having such a length value is applied, an aerogel composition having more excellent characteristics can be prepared over a wide area.

When the smaller value of the x-direction length value and the y-direction length value of the substrate 10 inserted into the substrate storage portion 20 is the "base material reference value", the x direction of the substrate storage portion 20 corresponding thereto The smaller of the length value and the y-direction length value, that is, the "length value of the substrate receiving portion" may be 1.00 to 3.00 times the reference value of the substrate, specifically 1.05 to 2.5 times, and more specifically, It can be 1.05 times to 2.0 times. The length of the substrate storage section corresponding to the reference value of the substrate storage section 20 and the substrate When the value is 3.00 times or more, the substrate 10 cannot be sufficiently supported by the substrate accommodating part 20, and when it is less than 1.00 times, the impregnation of the sol solution is insufficient. In addition, when the length of the substrate containing portion 20 and the reference value of the substrate are compared and the corresponding length value is 1.05 to 2.0 times, it is advantageous to prepare an aerogel composition having a flat surface and a fixed surface property.

The separation portion 30 may be in the form of a wall, and the upper and lower ends of the substrate receiving portion 20 are open.

The separation portion 30 may be in the form of a column including a front surface, a left side, a back surface, and a right side. The base material receiving portion 20 is a space surrounded by the separation portion 30 in the shape of a column, and its upper and lower ends are open.

The separation portion 30 may be a partition wall, and blocks fluid from moving between the first substrate receiving portion 20 and the second substrate receiving portion 20 in the x direction or the y direction.

The separation portion 30 may be mesh-shaped or have a plurality of holes, allowing the fluid to move between the first substrate receiving portion 20 and the second substrate receiving portion 20 in the x direction or the y direction.

The substrate support device 100 can be connected to a pressure reduction device that decompresses the substrate storage portion 20.

The substrate supporting device 100 may further include a lower end portion (not shown) for supporting the substrate supporting device 100 and the substrate 10 accommodated in the substrate supporting device at a lower end of the substrate supporting device 100, and the lower end portion allows fluid to the substrate. The lower end of the accommodating portion 20 moves in the z direction. Specifically, the receiving portion 20 may have a mesh shape or have a plurality of openings.

The fluid containing section is controlled by an external pressure reducing device 600, and the air density, that is, the air pressure, of the substrate containing section 20 can be adjusted, and in particular, the pressure can be reduced.

The lower support part 400 can move the supplied sol solution or cleaning solution to Substrate receiving section 20.

In the substrate supporting device 100, the substrate accommodating portion 20 may have an open upper end.

The substrate supporting device 100 may further include an upper end portion (not shown) located on the open upper end thereof, and the upper end portion allows the fluid to move toward the substrate receiving portion 20 in the z direction.

The upper end portion can move the supplied sol solution or cleaning solution to the substrate storage portion 20.

The substrate supporting device 100 may be connected to a solution recovery unit 700 that recovers the supplied sol solution or cleaning solution.

Hereinafter, a method of using the plate-shaped aerogel composition preparation device or the plate-shaped aerogel composition preparation substrate supporting device will be described.

The above-mentioned substrate supporting device is manufactured by preparing a plurality of separation sections in the form of a wall or a column, and arranging them so as to have appropriate substrate accommodating sections. In this case, in the case of a column-shaped separation section, it is only necessary to arrange the separation section having an appropriate substrate storage section side by side, and in the case of a wall-shaped separation section, it is disposed so as to have an appropriate substrate storage section. . In this case, it may be more convenient to use a front surface portion, a rear surface portion, or both the front surface portion and the rear surface portion in which a storage groove is formed in order to more easily form an appropriate substrate storage portion space between the separation portions. A substrate receiving portion is formed on the ground. A bonding unit to which a plurality of separation sections arranged as described above are fixed can be applied.

Such a separation portion may be arranged in the chamber, and such a separation portion may be arranged on a lower end support portion provided in the chamber. In this case, when an insertion groove is formed in a portion of the lower support portion that positions the separation portion, such a separation portion can be more easily disposed. In addition, such a separation part can be moved into the chamber in a state of being combined by a coupling unit after the configuration is completed outside the chamber. At this time, a separation portion may be disposed on the lower end support portion which is separately formed from the chamber. In this case, the lower end support portion and the lower end support portion are disposed. The upper separation part can be moved into the chamber together.

The substrate supporting device performs the process of inserting the substrate into the substrate supporting device before moving to the chamber or after being disposed in the chamber, and thereafter, an upper end fixing portion is selectively provided.

A sol solution is supplied to a substrate accommodated in a substrate supporting device to prepare an impregnated substrate whose substrate is impregnated with the sol solution.

The sol solution can be supplied from the upper end of the substrate, or the sol solution can be directly connected to the solution supply portion and the substrate supporting device. The solution supply portion is connected to the upper fixing portion, and the sol solution can be supplied to the substrate through the fluid receiving portion of the upper fixing portion. The upper end of the storage portion moves to impregnate the substrate.

At this time, the lower support portion may be connected to the pressure reducing device, and the impregnation may be performed sufficiently while the sol solution is supplied or after the sol solution is supplied, and the air bubbles between the fibers may be removed. In addition, the effect of preventing the collapse of the nanostructure formed by the sol solution can also be obtained by such a reduced pressure.

After the impregnation process of the sol solution is completed as described above, an aging (aging) process for achieving gelation may be performed. During the aging process or after the aging process is sufficiently performed, the substrate (the gelled substrate) is separated from the substrate supporting device.

Even if such separation occurs, the substrate (gelated substrate) has been gelled to a certain extent and its volume is increased compared to the substrate that was originally inserted, and it is stably located in the chamber similar to that before separation from the substrate support device. .

Since the upper or lower end of the substrate supporting device is open, the substrate (gelated substrate) can be easily separated from the substrate by passing the opened upper or lower end.

Solvent removal in the chamber of the substrate support device as described above Division process. This solvent removal process is a process of removing the solvent included in the gelled substrate and turning the wet gel into an aerogel. If necessary, i) directly perform the solvent removal process, ii) perform the reorganization and the solvent removal process, iii) performing cleaning and solvent removal processes, or iv) performing cleaning, reorganization and solvent removal processes.

Specifically, when cleaning is required, the cleaning and drying process can be performed by supplying a cleaning solution from a solution supply unit, and when reorganization is required, the reorganization and drying can be performed by supplying a reconstituted solution from a solution supply unit. Process. At this time, the aerogel may be hydrophobized while the cleaning solution includes the recombination solution.

The cleaning solution (or reconstituted solution) can be injected and supplied from the upper or lower direction of the substrate (gelated substrate), and the remaining cleaning solution (or reconstituted solution) can be moved to the lower support portion or the solution storage portion connected to the chamber. Then, it is discharged or re-transmitted to the solution supply unit for reuse.

Hereinafter, another method of using the plate-shaped aerogel composition preparation device or the plate-shaped aerogel composition preparation substrate supporting device will be described.

The process of arranging the fixed separation part in the substrate supporting device is the same as the above. However, at this time, the separation part is applied as a separation part having a net shape or having a plurality of openings, which can move the fluid in the x direction and the y direction. In addition, a lower end portion and an upper end portion that allow the fluid to move in the z direction are provided at the lower end and the upper end of the substrate supporting device, respectively.

In the case where a fluid-movable separation portion is also applied as described above, and a lower end portion and an upper end portion that are capable of moving the fluid are also provided, the substrate is located in the internal space of the substrate support portion to support it, but the solution or air Move in x, y, and z directions. In this case, the entire sol solution can be supplied to the inside of the chamber to perform the decompression process. In addition, after the gelation process has progressed to a certain degree, the solvent can also be performed without changing the chamber. Removal process, but for process efficiency, the substrate support device can be moved to another cleaning container or solvent removal container (or solvent removal device) to perform the solvent removal process, and the cleaning and recombination process can be performed as needed. At this time, the substrate supporting device is fluidly permeable all around except the upper end and the lower end. Therefore, the cleaning, recombination, and drying processes can be performed directly without removing the substrate supporting device.

A method for preparing a plate-like aerogel composition according to another embodiment of the present invention includes an impregnation step of supplying a sol solution to a substrate supporting device to prepare a plate-like substrate located in a substrate receiving portion and impregnated with the sol solution. That is, the substrate is impregnated. The substrate supporting device includes two or more substrate storage sections and separation sections, and a plate-shaped substrate is stored in the substrate storage section. The two or more substrate storage sections are as follows. A plate type having an x-direction length, a y-direction length, and a z-direction length. The z-direction length value is greater than the x-direction length value or the y-direction length value. The separation section spatially distinguishes adjacent substrate storage sections; An aging step to induce gelation and maturation of the sol solution contained in the impregnated substrate to prepare a gelled substrate; a device removal step to remove the gelled substrate from the open upper or lower end of the substrate containing portion A substrate supporting device; and a solvent removing step to remove the solvent from the gelled substrate to prepare an aerogel composition.

The description of the substrate, the substrate accommodating portion, the substrate supporting device, and the like are the same as those described above, and therefore, detailed descriptions thereof are omitted, and the above contents are included in the description of the method for preparing the plate-shaped aerogel composition.

The substrate can be a plate type fabric, a non-woven fabric, a net, or a laminate thereof having a length in the x direction, a length in the y direction, and a length in the z direction. In this case, a plate-shaped aerogel mat, Aerogel tablets and so on.

The substrate can be used alone or in combination with a sheet substrate to form an aerogel composition Foams, adhesives, fibers, cotton-like fiber aggregates, etc. In this case, aerogel compositions can be prepared according to the size and shape of the substrate storage portion. Specifically, plate-shaped aerogels can be prepared. Gel sheet, aerogel panel, aerogel felt, etc.

As the material of the substrate, for example, any one selected from the group consisting of inorganic fibers, organic fibers, and combinations thereof can be applied. The inorganic fiber may include any one selected from the group consisting of glass fibers, glass wool, rock wool, ceramic wool, boron fibers, and combinations thereof. One. The organic fiber may include a fiber selected from the group consisting of nylon, aromatic polyamide fibers, carbon fibers, polypropylene fibers, polyethylene fibers, polyester fibers, polyurethane fibers, acrylic fibers, polyvinyl chloride fibers, and fluorene fibers. , Regenerated fibers, waste fibers, cotton fibers, flax fibers, and combinations thereof.

The substrate is sufficiently impregnated with the sol solution due to its porosity, and functions as an aerogel support through the gelation process. The diameter of the fiber included in the substrate is 0.01 μm to 200 μm, and specifically, may be 0.01 μm to 100 μm, 0.05 μm to 50 μm, or 0.1 μm to 20 μm. The length of the fiber is 0.1 mm to 500 mm, and specifically, may be 0.1 mm to 100 mm, 0.2 mm to 200 mm, or 0.5 mm to 50 mm, but is not limited thereto.

Specifically, as the base material, glass fiber fabric or ceramic wool can be applied.

The substrate inserted into the substrate receiving portion in the impregnation step may be one that satisfies the following conditions: the smaller of the x-direction length and the y-direction length of the substrate is the reference value, and the length value of the corresponding substrate receiving portion It is 1.05 times to 3.00 times, 1.2 times to 2.5 times, and more specifically 1.4 times to 2.0 times the reference value.

The sol solution may be selected from the group consisting of zirconia, yttrium oxide, hafnium oxide, oxygen A solution of a precursor of any one of the group consisting of aluminum oxide, titanium oxide, cerium oxide, silicon oxide, magnesium oxide, calcium oxide, magnesium fluoride, and calcium fluoride. In this case, the solvent can be selected and applied according to the characteristics of the precursor included in the solution.

Specifically, as the sol solution, a silica-based sol solution can be applied, and more specifically, any one selected from the group consisting of a sodium silicate solution called water glass, a potassium silicate solution, and a combination thereof can be applied. .

The impregnation may be performed by supplying the sol solution to the substrate containing portion or the chamber and leaving it to stand. This impregnation process may be performed for 10 minutes to 2 hours, and more specifically, for 10 minutes to 1 hour. In this case, when the pressure is reduced by the pressure-reducing device in the substrate storage portion or the chamber, the impregnation can be performed more quickly.

The aging step is a process of preparing a gelled substrate formed by gelation and aging of the sol solution contained in the impregnated substrate prepared in the impregnation step.

The gelation can be performed under the conditions of the catalyst. In this case, an acid catalyst can be used as the catalyst, and specifically, a sulfuric acid solution, a hydrochloric acid solution, or an acetic acid solution can be used.

The aging step can be performed in a state in which the space in the substrate accommodating section, the substrate supporting device, or the chamber including the substrate accommodating section is reduced to 300 Torr or less by a decompression device. Specifically, the pressure can be reduced in a range of 0.001 Torr to 300 Torr, 0.001 Torr to 100 Torr, or 0.001 Torr to 10 Torr. When the sol is impregnated into the base material under such reduced pressure, air bubbles generated by the surface tension of the fibers included in the base material can be effectively removed. In addition, the collapse of the nanostructure formed on the impregnated substrate due to gelation can be minimized by this reduced pressure.

This decompression can be maintained for 10 minutes to 2 hours and for 10 minutes to 1 hour.

In the aging step, it is formed in order to sufficiently gel the impregnated substrate. The nanostructure can be aged at a normal temperature and a temperature of 40 ° C to 80 ° C for 2 to 48 hours to perform the aging process, and can be left to stand at a temperature of 40 ° C to 60 ° C for 4 to 24 hours to perform the aging process. Compared with the impregnated base material, the gelled base material formed by curing as described above has a stronger nanogel structure.

The device removal step separates the gelled substrate having such a relatively strong nanogel structure from the substrate supporting device. In the case where an ordinary partition-like material other than the fluid-permeable material is used as the separation part of the substrate supporting device, in order to efficiently perform the subsequent solvent removal step, such a substrate may be performed before the solvent removal step is performed. Supports separation of devices.

During the impregnation step and the aging step, most of the sol solution on the substrate becomes a gel of a relatively hard structure, so that the nanostructure is not excessively damaged or collapsed during the separation process of the substrate supporting device.

As described above, the gelled substrate separated from the substrate supporting device is subjected to a solvent removal step in the same chamber to prepare an aerogel composition.

The solvent removal step is a process of removing the solvent in the nanostructure without collapsing the gel structure or minimizing the collapse, and may be a normal temperature process or a process using a supercritical fluid.

Specifically, the solvent removing step may further include a cleaning process. In the case of cleaning at normal temperature, the cleaning may be sequentially performed 1 cleaning, 2 cleanings, and 3 cleanings, and 1 cleaning application includes 1 cleaning of distilled water Liquid, the secondary cleaning application includes a secondary cleaning solution of acetone, and the third cleaning application includes a three cleaning solution of an alcohol selected from the group consisting of propanol, butanol, and combinations thereof. This cleaning is a process of removing excess ions remaining on the gelled substrate and exchanging the solvent present in the gelled substrate.

The solvent removal step further includes a recombination process. The recombination can be performed by applying a recombination solution including an organic solvent and a silane compound in a weight ratio of 1: 0.1 to 1: 1 to the cleaned gelled substrate. As the organic solvent included in the reconstituted solution, any one selected from the group consisting of hexane, toluene, xylene, and a combination thereof can be applied, and the silane compound can be applied selected from the group consisting of trimethylchlorosilane (TMCS) and hexamethyldisila Any of the groups consisting of azamethane (HMDS), dimethylchlorosilane (DMCS), methyltrichlorosilane (MTCS), and combinations thereof. Specifically, the recombination solution may include hexane and trimethylchlorosilane.

The recombination solution can include an organic solvent and a silane compound in a weight ratio of 1: 0.1 to 1: 1, a weight ratio of 1: 0.1 to 1: 0.5, and a weight ratio of 1: 0.2 to 1: 0.4. When a silane compound is used together with an organic solvent at such a content, it is possible to fully recombine and reduce waste of medicines.

The solvent removing step is a process (drying process) of removing the solvent from the gelled substrate, and can be applied to the gelled substrate, the gelled substrate after the cleaning process, or the gelled substrate after the recombination step. The solvent removal step can be performed by normal pressure drying, supercritical drying, or alternately by normal pressure drying and supercritical drying.

Drying under normal pressure may be performed at 5 ° C to 350 ° C for 60 minutes to 600 minutes, or at 20 ° C to 250 ° C for 60 minutes to 240 minutes. Supercritical drying can be performed using carbon dioxide as a supercritical fluid under temperature conditions of about 40 ° C to 150 ° C and pressure conditions of 75 bar to 800 bar.

In the case of drying in a normal pressure drying method, specifically, in the solvent removal step, the reconstituted gelled substrate may be washed with hexane, and then dried in an air environment at 5 ° C to 350 ° C for 60 minutes. To 600 minutes.

Utilization of pure water of aerogel composition prepared in this way The measured contact angle may be 95 degrees to 170 degrees, 110 degrees to 160 degrees, and it may be one having excellent hydrophobicity with a contact angle of 110 degrees to 130 degrees.

A method for preparing a plate-shaped aerogel composition according to still another embodiment of the present invention includes an impregnation step of accommodating a plate-shaped substrate on a plate-shaped lower end portion of a substrate-supporting device having a fluid permeability, so as to have a fluid. The permeable upper end portion fixes the upper end of the substrate support device and supplies a sol solution to prepare a plate-shaped substrate located in the substrate receiving portion and impregnated with the sol solution, that is, an impregnated substrate. The substrate support device includes two or more substrates. Material storage section and fluid-permeable separation section, and the two or more substrate storage sections are spaces that have a plate type having a length in the x direction, a length in the y direction, and a length in the z direction, and a length in the z direction The value is greater than the length value in the x direction or the length value in the y direction. The fluid-permeable separating portion spatially distinguishes adjacent substrate storage portions. The aging step induces gelation and aging of the sol solution contained in the impregnated substrate. And preparing the gelled substrate; the device moving step moves the substrate support device to the solvent removal device, and the substrate support device includes the gelled substrates located in the substrate containing section and includes each other Separating bonded portion, upper portion and lower portion; and a solvent removal step, the solvent was removed gelation device included in the base composition was prepared in the airgel the solvent removed.

The description of the above-mentioned substrate, the substrate storage portion, the substrate support device, and the like are the same as those described above. Therefore, detailed descriptions thereof are omitted, and the above-mentioned contents are included in the description of the method for preparing the plate-shaped aerogel composition.

Specific descriptions regarding the impregnation step, the aging step, the solvent removal step, and the constituent elements included in each step are the same as those described in the method for preparing the above-mentioned plate-shaped aerogel composition. Therefore, the description is omitted, and Included in the description of the method for preparing the plate-like aerogel composition.

The device moving step is a process of moving the substrate supporting device from the chamber to the solvent removing device. When the plate-shaped aerogel composition is prepared by applying the device moving step as described above, the separation part of the substrate supporting device and the like continuously fix the substrate supporting each step during the process of preparing the aerogel composition. Therefore, damage to the nanostructure of the aerogel that may occur is minimized, and an aerogel composition can be prepared. In addition, two types of reactors, such as a chamber for carrying out the impregnation process and a solvent removing device, are used. Therefore, compared with the case where all the steps are performed in one chamber, the sol solution is recovered, or the case where cleaning or recombination is performed The recovery of the solution or the reconstituted solution is relatively easy, and it is assumed that when the aerogel composition is prepared by a continuous process, the preparation efficiency can be further improved.

As mentioned above, the preferred embodiments of the present invention have been described in detail, but the scope of patent application of the present invention is not limited to this. The industry uses various modifications and basic concepts of the present invention as defined in the scope of the following patent application for invention. The improved form also falls within the scope of the patent application of the present invention.

Claims (20)

A plate-shaped aerogel composition preparation device includes: i) a substrate supporting device, including a first substrate accommodating portion, a second substrate accommodating portion, and a separation portion; There are two or more substrates divided in the upper section. The first substrate accommodating part is used for accommodating the first substrate, and has a plate shape having a length in the x direction, a length in the y direction, and a length in the z direction. The length value in the z direction is greater than the x direction. A length value or a length value in the y direction, the second substrate receiving portion is adjacent to the first substrate receiving portion, is spatially distinguished from the first substrate receiving portion, and contains a second substrate, and The separation portion is located between the first substrate receiving portion and the second substrate receiving portion to distinguish two spaces, and includes a substrate receiving portion including the first substrate receiving portion and the second substrate receiving portion. The lower or upper end of the portion is open; ii) a chamber that houses the substrate support device therein; and iii) a solution supply portion that supplies a sol solution or a cleaning solution to the substrate accommodation portion, wherein the z-direction is from An upper end of the substrate receiving portion extends toward a lower end of the substrate receiving portion. Direction and the x direction and the y-direction are perpendicular to the z-direction, and the direction perpendicular to the x y direction. The plate-shaped aerogel composition preparation device according to item 1 of the scope of the patent application, wherein the separation portion is in the form of a wall, and the upper end and the lower end of the substrate receiving portion are open. The device for preparing a plate-shaped aerogel composition according to item 1 of the scope of patent application, wherein the separation portion is a column shape including a front surface, a left surface, a back surface, and a right surface, and the substrate storage portion is surrounded by all parts. In the space surrounded by the separation portion in the column shape, the upper end and the lower end of the substrate receiving portion are open. The plate-shaped aerogel composition preparation device according to item 1 of the scope of the patent application, wherein the separation portion is a partition wall shape and blocks fluid between the first substrate receiving portion and the second substrate receiving portion. Move in the x or y direction. The plate-shaped aerogel composition preparation device according to item 1 of the scope of patent application, wherein the separation portion is mesh-shaped or has a plurality of openings, allowing fluid to flow between the first substrate receiving portion and the second The substrate accommodating portions move between the x direction and the y direction. The device for preparing a plate-shaped aerogel composition according to item 1 of the scope of the patent application, further includes a decompression device for decompressing the substrate storage portion. The device for preparing a plate-shaped aerogel composition according to item 2 or item 3 of the scope of patent application, further comprising a lower end supporting portion located at a lower end of the substrate supporting device to support the substrate supporting device, said The lower end support portion allows a fluid to move in a z direction between one surface of the lower end support portion and a lower end of the substrate receiving portion. The plate-shaped aerogel composition preparation device according to item 2 or item 3 of the patent application scope, wherein the substrate receiving portion has an open upper end, and an upper end fixing portion is further included on an upper portion of the substrate supporting device. . The plate-shaped aerogel composition preparation device according to item 8 of the scope of application for a patent, wherein the upper end fixing portion further includes a fluid containing portion for containing a sol solution or a cleaning solution supplied by the solution supply portion to make it Move to the said substrate storage part. The apparatus for preparing a plate-shaped aerogel composition according to item 1 of the scope of the patent application, further includes a solution recovery unit for recovering the sol solution or the cleaning solution supplied to the substrate supporting device. A substrate support device for preparing a plate-like aerogel composition, which divides a space by a separation portion, and divides and stores two or more substrates in space, including: a first substrate storage portion, which houses the first substrate, It has a plate shape having a length in the x direction, a length in the y direction, and a length in the z direction, and the length value in the z direction is greater than the length value in the x direction or the length in the y direction; a second substrate receiving portion is adjacent to the first substrate receiving portion Is spaced apart from the first substrate receiving portion and accommodates a second substrate in space; and a separation portion is located between the first substrate receiving portion and the second substrate receiving portion to distinguish two spaces. Wherein the lower or upper end of the substrate accommodating portion including the first substrate accommodating portion and the second substrate accommodating portion is open, and the z direction is from the upper end of the substrate accommodating portion to the base. The direction in which the lower end of the material receiving portion extends, and the x direction and the y direction are both perpendicular to the z direction, and the x direction is perpendicular to the y direction. According to the substrate supporting device for preparing a plate-shaped aerogel composition according to item 11 of the scope of application for a patent, the separation portion is in the form of a wall, and an upper end and a lower end of the substrate receiving portion are open. The substrate supporting device for preparing a plate-shaped aerogel composition according to item 11 of the scope of application for a patent, wherein the separation portion is a column shape including a front surface, a left surface, a back surface, and a right surface, and the substrate storage portion It is a space surrounded by the said separation part of the said column shape, The upper end and the lower end of the said base material accommodation part are open. The substrate support device for preparing a plate-shaped aerogel composition according to item 11 of the scope of application for a patent, further comprising a lower end portion, which is located at a lower end of the substrate support device for preparing a plate-shaped aerogel composition and supports storage. The substrate to the substrate accommodating portion allows the fluid to move in the z direction. The substrate supporting device for preparing a plate-like aerogel composition according to item 11 of the scope of application for a patent, wherein the substrate receiving portion has an open upper end, and the substrate-like support for preparing the plate-like aerogel composition The device further includes an upper end portion located on the open upper end of the substrate accommodating portion, allowing the fluid to move in the z direction. A method for preparing a plate-shaped aerogel composition includes an impregnation step of supplying a sol solution to a substrate support device to prepare a plate-shaped substrate located in a substrate receiving portion and impregnated with the sol solution, the plate-shaped The substrate is an impregnated substrate, and the substrate supporting device includes two or more substrate receiving portions and separation portions, and the plate-like substrate is accommodated in the substrate receiving portion, and two or more substrates are accommodated. The substrate accommodating portion has a plate shape having an x-direction length, a y-direction length, and a z-direction length. The z-direction length value is greater than the x-direction length value or the y-direction length value. The separation portion spatially distinguishes each other from each other. In the adjacent substrate accommodating portion, the z direction is a direction extending from an upper end of the substrate accommodating portion to a lower end of the substrate accommodating portion, and the x direction and the y direction are perpendicular to each other. The z direction and the x direction are perpendicular to the y direction; an aging step, which induces gelation and aging of the sol solution contained in the impregnated substrate to prepare a gelled substrate; a device removal step Through the open upper part of the substrate receiving part Or from the lower end of the base support means for removing gelled said substrate; and a step of removing the solvent from the gel and airgel substrate removal of the solvent composition. A method for preparing a plate-like aerogel composition includes an impregnation step of accommodating a plate-like substrate on a plate-like lower end portion of a substrate-supporting device having fluid permeability, and then using a fluid-permeable upper end portion. The upper end of the substrate supporting device is fixed to supply a sol solution to prepare the plate-shaped substrate that is located in the substrate containing portion and is impregnated with the sol solution. The plate-shaped substrate is an impregnated substrate. The material supporting device includes two or more of the substrate accommodating portion and a fluid-permeable separation portion. The two or more substrate accommodating portions are plate-shaped and have a length in the x direction, a length in the y direction, and a length in the z direction. , The z-direction length value is greater than the x-direction length value or the y-direction length value, and the separation portion having fluid permeability spatially distinguishes the substrate containing portions adjacent to each other, wherein the z direction is from the base A direction in which an upper end of the material receiving portion extends toward a lower end of the substrate receiving portion, and the x direction and the y direction are perpendicular to the z direction, and the x direction is perpendicular to the y direction; an aging step To induce the impregnated base The sol solution contained in the gel solution is gelled and aged to prepare a gelled substrate; a device moving step moves the substrate support device to a solvent removal device, and the substrate support device includes the substrate The gelled base material in the containing portion, and including the separation portion, the upper end portion, and the lower end portion combined with each other; and a solvent removing step, in the solvent removing device, from the gelation The solvent is removed from the substrate to prepare an aerogel composition. The method for preparing a plate-like aerogel composition according to item 16 or item 17 of the scope of patent application, wherein the aging step is to place the substrate receiving portion or the substrate supporting device by a pressure reducing device. The internal pressure was reduced to 300 Torr or less. The method for preparing a plate-shaped aerogel composition according to item 16 or item 17 of the scope of application for a patent, wherein the substrate accommodating portion is smaller in the x-direction length value or the y-direction length value. When the value of is a reference value, the z-direction length value has a value that is 5 times or more the reference value. The method for preparing a plate-shaped aerogel composition according to item 16 or item 17 of the scope of application for a patent, wherein the substrate inserted into the substrate accommodating part in the impregnation step is based on the The smaller of the x-direction length and the y-direction length is a reference value, and the smaller of the x-direction length and the y-direction length of the substrate containing portion corresponding to the substrate is 1.00 times the reference value. To 3.00 times.