TWI688690B - Method for preparing aerogel composites and apparatus therefor - Google Patents

Abstract

Embodiments are capable of providing an apparatus for preparing an aerogel composite, which comprises a container; a core fixing device provided inside the container; and a core engageable with the core fixing device, and a process for preparing an aerogel composite using the same.

Description

Method and device for preparing aerogel composite material

Field of the Invention The embodiments relate to a method and apparatus for preparing an aerogel composite material without a separator.

BACKGROUND OF THE INVENTION Aerogel is the lightest solid developed by humans and is a super-insulating material with a porosity of more than about 95%. Aerogel is already a highly anticipated novel material as an insulating material and sound insulation material in the future. In recent years, R&D personnel have actively used it in various industrial fields. In general, aerogels have low density, open pore structure, large surface area, and nanometer pore size.

In order to improve the processability when preparing these aerogels, attempts have been made to use the conveyor belt dipping method (see Korean Patent No. 1133025 and FIG. 1). However, in the conventional conveyor belt dipping method, an appropriate viscosity is required to prevent the loss of sol flow. Impregnation of a sol with a high viscosity may cause bubbles in the aerogel, thereby weakening its performance. In order to solve this problem, it is necessary to reduce air bubbles and provide sufficient transfer time for uniform impregnation. However, this may reduce the yield, because the length of the conveyor belt needs to be longer, and the burrs generated in the pressing roller step must be removed. Furthermore, in the conveyor belt dipping method, the reaction should occur during the transfer to the extent that the sol is sufficiently gelatinized and thus the product produced can be rolled up. However, there is a limitation that the gelation time required for producing high-quality nano-scale pores cannot be sufficiently given.

In addition, according to the conventional method, although the sol is treated by dipping after its viscosity has been reduced, the amount of sol is insufficient to some extent or the sol is uneven to some extent. Therefore, additional sol must be injected into the aging tank to compensate for the insufficient sol. As a result, some of the resulting aerogels will be released and scattered in the form of powder, which is considered a serious problem in its construction and will lose its performance quality.

In addition, in the case where the separator is used to separate the composite material after gelation into a roll form, additional steps must be performed, such as inserting the separator before sol impregnation and removing the separator before the post-gelation cleaning step, which results in efficiency Reduce the problem.

Technical Problem In order to prepare a composite material in which an aerogel is formed, the purpose of the embodiments is to provide an economical method for preparing an aerogel composite material, which uses a batch procedure instead of a continuous procedure, and a natural separation method using a fibrous substrate, Instead of using partitions, and a device for this method. Solution to the problem

An apparatus for preparing an aerogel composite material according to an embodiment includes: a container; a core fixing element provided in the container; and a core, which can be engaged with the core fixing element.

An apparatus for preparing an aerogel composite material according to another embodiment includes: a container; a core fixing element provided in the container; a substrate fixing element provided in the container; and a core Body, which can be engaged with the core fixing element, wherein the container, the core or both are rotatable.

The method for preparing an aerogel composite material according to an embodiment includes: (A) winding a fiber substrate on a core; (B) placing the core wound with the fiber substrate on a (C) inject a sol into the container and impregnate it into the fibrous substrate; (D) seal the container, defoam the sol by changing the pressure, and gel the sol; and (E) Inject a surface treatment solution into the container and dry the fiber substrate.

A method for preparing an aerogel composite material according to another embodiment includes: (A) winding a fiber substrate on a core; (B) placing the core wound with the fiber substrate In a container; (B') joining one end of the wound fiber substrate to a substrate fixing element provided in the container; (C) injecting a sol into the container and impregnating the fiber substrate (D) seal the container, defoam the sol by changing the pressure, and gel the sol; (D') rotate the container, the core or both; and (E) in the container Inject a surface treatment solution and dry the fiber substrate.

In addition, the aerogel composite material is prepared by the method for preparing an aerogel composite material described above. Advantageous effects of the invention

According to the device for preparing an aerogel composite material and the method for using the device for preparing an aerogel composite material according to this embodiment, a low thermal conductivity and a low thermal conductivity can be produced without a separator and regardless of the viscosity of the sol Aerogel composite material with improved thermal insulation performance.

In addition, according to the preparation method described above, the method is economical because it can produce aerogel composite materials in a simpler and more convenient manner.

Best Mode for Carrying Out the Invention Hereinafter, the present invention will be explained in detail with reference to examples. As long as the essence of the present invention is not changed, these examples can be modified into various forms.

The upper and lower relationship of each component will be explained with reference to the drawings. In the drawings, the same symbol number means the same unit, and the size and thickness of each unit may be enlarged for convenience of explanation.

In this specification, when a component is referred to as "including" a unit, it should be understood that the component may also include other units.

Furthermore, all numbers used herein to indicate the number of components, reaction conditions, etc., should be understood as modified by the term "about". Device for preparing aerogel composite material

The apparatus for preparing aerogel composite materials according to an embodiment is an apparatus that can economically prepare aerogel composite materials using a batch method without a separator.

The device (11, 12, 13) for preparing an aerogel composite material according to an embodiment includes: a container (1); a core fixing element (2) provided in the container; and a core (3), which can be engaged with the core fixing element. In this case, the container, the core or both can be reduced or enlarged (see Figures 1 and 2).

FIG. 1 depicts an apparatus for preparing aerogel composite materials by using the reduction of the core. Figure 2 depicts an apparatus for making aerogel composites using the expansion of a container.

In FIGS. 1 and 2, a1 is the diameter of the core before the core is reduced, a2 is the diameter of the core after the core is reduced, b1 is the diameter of the container before the expansion of the container, and b2 is the diameter of the container after the expansion of the container. Here, a1 is larger than a2, and b1 is smaller than b2.

The core fixing element (2) and the core (3) are separately separable from the container (1).

The material of the container (1) is not particularly limited, but it can be made of a chemically resistant material. Specifically, stainless steel materials, coated metal materials, or glass may be used.

The shape of the container is not particularly limited, but it may be cylindrical according to the shape of the fibrous substrate wound around the core. In addition, the size of the container is not particularly limited, and it can be appropriately selected depending on the size of the fiber base material wound around the core.

The material of the core fixing element (2) is not particularly limited, but it can be made of a chemically resistant material. Specifically, stainless steel materials, coated metal materials, or glass may be used.

The core can be fixed to the lower part of the container through the core fixing element. Specifically, it can be vertically fixed to the lower part of the container. More specifically, it can be vertically fixed to the lower part of the middle of the container. But it is not limited to this.

The core fixing element (2) is rotatable. Specifically, when the core is fixed, the core fixing element can rotate about the central axis in the longitudinal direction of the core.

The material of the core (3) is not particularly limited, but it can make the material chemically resistant. Specifically, stainless steel materials, coated metal materials, or glass may be used.

The shape of the core may be cylindrical, but it is not limited thereto.

The container, the core, or both contain multiple fragments. Alternatively, the container, the core, or both may be composed of multiple fragments.

The container, the core, or both may shrink or expand as adjacent ones of the plurality of fragments are spaced apart or overlap.

Optionally, the container, the core, or both may shrink or expand as adjacent ones of the plurality of fragments are spaced apart or meet.

Optionally, the container, the core, or both may shrink or expand as adjacent ones of the plurality of fragments meet or overlap.

The core is shrinkable in the center direction of the core.

Specifically, the core may be composed of a fixed core member (101a, 101b) and a plurality of fragments (102a, 102b) surrounding the fixed core member. In this case, the plurality of fragments (102a) are spaced apart from each other around the fixed member, and the core can then shrink as the plurality of fragments (102b) adjacent to each other meet or overlap (see Figure 3).

In addition, the core may be composed of multiple fragments. In this case, the plurality of fragments are spaced apart from each other, and the core may then shrink as the plurality of fragments adjacent to each other meet or overlap. Optionally, the plurality of fragments are in contact, and the core may then shrink as the plurality of fragments adjacent to each other overlap (see FIG. 5).

As another example, the core may be in the form of a winding roll, and may be reduced or enlarged as the interval between the winding materials is adjusted.

As another example, the core includes a fixed core member and a partition member around the fixed core member, and it can be reduced by removing the partition member.

The cross-sectional area of the core body after the core body is reduced in the center direction of the core body may be 5 to 90% of the cross-sectional area of the core body before the core body is reduced. Specifically, the cross-sectional area of the core after the core is reduced in the central direction of the core may be 5 to 70%, 10 to 60%, or 10 of the cross-sectional area of the core before the core is reduced To 50%, but not limited to this.

The cross-sectional area of the core means the cross-sectional area perpendicular to the longitudinal direction of the core.

For example, referring to FIG. 3, the cross-sectional area of the core before reduction means the area of a circle with a diameter a1, and the cross-sectional area of the core after reduction means the area of a circle with a diameter a2. Here, a1 is greater than a2.

The cross-sectional area of the core is 1 to 40% of the internal cross-sectional area of the container. Specifically, the cross-sectional area of the core may be 5 to 35%, 5 to 30%, or 10 to 25% of the internal cross-sectional area of the container, but is not limited thereto.

The core may also expand in the opposite direction to the center of the core. That is, the core can be reduced or enlarged. Therefore, it is economical because the device is reusable.

The container is expandable in the opposite direction to the center of the core.

Specifically, the container may be composed of a fixed container wall (103a, 103b) and a plurality of fragments (104a, 104b). In this case, the plurality of fragments are in contact, and the container can then expand as the plurality of fragments (104b) adjacent to each other are spaced apart (see FIG. 4).

In addition, the container may be composed of multiple fragments. In this case, the plurality of fragments overlap each other, and the container can then expand as the plurality of fragments adjacent to each other meet (see FIG. 5).

As another example, the fixed container wall may be in the form of a winding roll, and may expand or contract as the interval between the winding materials is adjusted.

As another example, the container includes a fixed container wall and a partition wall, and the container can be reduced by removing the partition wall.

The cross-sectional area of the inside of the container after the expansion of the container may be 105 to 150% of the cross-sectional area of the container before the expansion of the container. Specifically, the cross-sectional area of the inside of the container after the expansion of the container may be 105 to 145%, 110 to 140%, or 110 to 130% of the cross-sectional area of the container before the expansion of the container, but is not limited thereto.

The cross-sectional area inside the container means the area of the inner circumference of the lower part of the container.

For example, referring to FIG. 4, the cross-sectional area of the inside of the container before expansion of the container means the area (105a) of a circle with a diameter b1, and the cross-sectional area of the inside of the container after expansion of the container means a circle with a diameter of b2 Area (105a). Here, b2 is greater than b1.

The container can also be reduced in the direction of the center of the core. That is, the container can be reduced or enlarged. Therefore, it is economical because the device is reusable.

The container, the core or both are rotatable.

The core can rotate around the central axis in the longitudinal direction of the core. In addition, the container can rotate about the central axis of the container.

When the container, the core or both are reduced or enlarged, the core can rotate around the central axis in the longitudinal direction of the core at the same time. In addition, when the container, the core, or both are reduced or enlarged, the container can simultaneously rotate around the central axis of the container.

The device for preparing an aerogel composite material may further include a substrate fixing element provided in the container. In this case, the substrate fixing element functions to fix one end of the fiber substrate.

An apparatus for preparing an aerogel composite material according to another embodiment includes: a container; a core fixing element provided in the container; a substrate fixing element provided in the container; and a core Body, which can be engaged with the core fixing element, wherein the container, the core or both are rotatable.

In the case where the container, the core or both are rotatable in an apparatus for preparing aerogel composite materials, the apparatus includes a substrate fixing element.

The substrate fixing element may be provided in the container. In particular, the substrate fixing element may be provided on the inner wall of the container. This function is to fix one end of the fiber substrate.

In the apparatus for preparing aerogel composite materials, the container, the core, or both can be reduced or enlarged. Specifically, the core can be reduced in the center direction of the core, and it can also be enlarged for repeated use. In addition, the container can be enlarged in the opposite direction to the center of the core, and it can also be reduced for repeated use.

For the details of the container, the core fixing element, the core, etc., refer to the above description.

Since the device for preparing aerogel composite materials is reusable and does not require unnecessary steps, the method for preparing aerogel composite materials is relatively economical. Method for preparing aerogel composite material

The method for preparing an aerogel composite material according to an embodiment includes: (A) winding a fiber substrate on a core; (B) placing the core wound with the fiber substrate on a (C) inject a sol into the container and impregnate it into the fibrous substrate; (D) seal the container, defoam the sol by changing the pressure, and gel the sol; and (E) Inject a surface treatment solution into the container and dry the fiber substrate. In addition, the method for preparing the aerogel composite material may further include: (D'') shrinking the core in the direction of the center of the core, or enlarging the container in the direction opposite to the center of the core. Here, this step (D'') may be performed after step (D).

1 and 2, a method for preparing an aerogel composite material according to an embodiment will be described below.

According to a method for preparing an aerogel composite material according to an embodiment, the "device for preparing an aerogel composite material" described above is used. Therefore, for details about the device used to prepare the aerogel composite material—that is, the container, the core fixing element, and the core—refer to the section above on “ Device for preparing the aerogel composite material ” Mentioned.

First, a fiber substrate is wound on a core (step (A)).

The fibrous substrate can be in the form of a long mat. For example, the fiber substrate may be a woven mat or a non-woven mat, but it is not limited thereto.

In addition, the fibrous base material may include only one or both of inorganic fibers and organic fibers.

The inorganic fiber may be at least one selected from the group consisting of glass fiber, glass wool, rock wool, ceramic wool, and boron fiber, but is not limited thereto.

The organic fiber may be at least one selected from the group consisting of nylon, Fanglun fiber, carbon fiber, polypropylene fiber, polyethylene fiber, polyester fiber, polyurethane fiber, acrylic fiber, poly Vinyl chloride acetate fiber, spiral fiber, regenerated fiber and waste fiber, but not limited to this. In addition to these fibers, you can also choose special fibers or general fibers used in daily life, such as cotton or linen.

The diameter of the fiber may be 0.01 to 200µm, especially 0.01 to 100µm, 0.05 to 50µm or 0.1 to 20µm, but it is not limited thereto. In addition, the length of the fiber may be 0.1 to 500 mm, particularly 0.1 to 100 mm, 0.2 to 200 mm, or 0.5 to 50 mm, but is not limited thereto.

A single layer to 100 layers of the fiber substrate may be wound on the core, but it is not limited thereto. Specifically, 2 to 50 layers of the fibrous substrate can be wound on the core. It is best to wind it appropriately according to the thickness of the fibrous base material and the size of the container.

Next, the core wound with the fiber substrate is placed in a container (step (B)).

Here, the core wound with the fiber base material can be placed in a container and joined with a core fixing element.

The core fixing element (2) is placed under the container, and the core (3) wound with the fiber base material (4) is vertically fixed through the core fixing element.

It is economical because the use of a core wound directly on the fiber substrate does not require any separate wetting pretreatment.

After that, a sol is injected into the container and immersed in the fibrous base material (step (C)).

The sol may be at least one selected from the group consisting of zirconium oxide, yttrium oxide, hafnium oxide, aluminum oxide, titanium dioxide, cerium oxide, silicon dioxide, magnesium oxide, calcium oxide, magnesium fluoride, and fluoride calcium.

Specifically, the sol may be a silica-based sol, but is not limited thereto.

In addition, the fiber substrate is impregnated for 10 minutes to 2 small pieces. Specifically, the fibrous substrate may be impregnated for 10 minutes to 1 hour.

Next, the container is sealed, and the sol is defoamed and gelled by changing the pressure (step (D)).

The step of changing the pressure means the step of pressurizing or depressurizing. Specifically, the container can be sealed and depressurized to defoam and gel the sol.

The container can be sealed and the pressure in the container reduced to a range of 0.001 to 300 Torr, 0.001 to 100 Torr, or 0.001 to 10 Torr absolute pressure.

By sealing the container and reducing the pressure in the container, the bubbles generated by the surface tension of the inorganic fiber or organic fiber when the sol is immersed in the fiber substrate can be effectively removed.

In addition to depressurization, sealing the container is also intended to prevent the gel structure from collapsing due to the drying of the contents of the container.

Furthermore, the defoaming can be performed for 10 minutes to 2 hours. Specifically, it can be performed for 10 minutes to 1 hour.

The sol impregnated into the fibrous substrate is then gelled and aged. Specifically, the gelled sol can be aged at normal pressure and a temperature of 40 to 80°C for 2 to 48 hours. Specifically, it may be aged at a temperature of 40 to 60°C for 4 to 24 hours, but it is not limited thereto.

Steps (C) and (D) can be repeated several times. For example, this step (C) and (D) can be alternately performed several times. More specifically, this step may be repeated in the order of steps (C), (D), (C), (D), and so on.

After that, the core body can be reduced in the center direction of the core body, or the container can be enlarged in the direction opposite to the center of the core body (step D'').

The core body can be reduced in the center direction of the core body as described in the apparatus for preparing an aerogel composite material.

In this case, the cross-sectional area of the core after the core is reduced may be 5 to 90% of the cross-sectional area of the core before the core is reduced. Specifically, the cross-sectional area of the core body after the core body is reduced may be 5 to 70%, 10 to 60%, or 10 to 50% of the cross-sectional area of the core body before the core body is reduced, but is not limited thereto .

The cross-sectional area of the core means the cross-sectional area perpendicular to the longitudinal direction of the core.

Alternatively, the container can be enlarged in the direction opposite to the center of the core as described in the apparatus for preparing an aerogel composite material.

In this case, the cross-sectional area of the inside of the container after the expansion of the container is 105 to 150% of the cross-sectional area of the inside of the container before the expansion of the container. Specifically, the cross-sectional area of the interior of the container after the expansion of the container is 105 to 145%, 110 to 140%, or 110 to 130% of the cross-sectional area of the interior of the container before the expansion of the container, but is not limited thereto.

When the core is reduced, the container, the core, or both can rotate simultaneously. In this case, the rotation direction of the core, the container, or both is the same as the winding direction of step (A). In this case, the winding roll can be separated more effectively.

Optionally, when the container is enlarged, the container, the core, or both can rotate simultaneously. In this case, the rotation direction of the container, the core, or both is the same as the winding direction of step (A). In this case, the winding roll can be separated more effectively.

When the core shrinks in the direction of the center of the core, or when the container expands in the direction opposite to the center of the core, the volume of space around the core around which the fiber base material is wound increases at this time, As a result, the fiber base material is further wound, thereby widening the inner layer spacing of the fiber base material. Because the inner layer spacing increases, solvent cleaning and surface treatment can be effectively performed, and materials filled in the gel gap can be effectively replaced with other solvents.

Next, a surface treatment solution is injected into the container, and then the fiber substrate is dried (step (E)).

The surface treatment solution is at least one selected from the group consisting of: distilled water; C ₁ -C ₈ alcohols, such as isopropanol; ketones, such as acetone; C ₁ -C ₁₂ alkanes, such as hexane; Aromatic solvents such as toluene, xylene, etc.; silane compounds such as trimethylchlorosilane (TMCS), hexamethyldisilazane (HMDS), dimethylchlorosilane (DMCS), methyltrichlorosilane (MTCS) etc.

Specifically, the surface treatment solution may be distilled water, acetone, isopropanol, hexane, TMCS, etc., but is not limited thereto.

The fibrous substrate can be washed 1 to 50 times with a surface treatment solution at 20 to 80°C.

The drying step may be atmospheric drying or supercritical drying.

The atmospheric drying is performed at 5 to 350°C for 60 to 600 minutes; or at 20 to 250°C for 60 minutes to 240 minutes.

Furthermore, the supercritical drying can be performed at about 100 to 200 atmospheres, but is not limited thereto.

A method for preparing an aerogel composite material according to another embodiment includes: (A) winding a fiber substrate on a core; (B) placing the core wound with the fiber substrate A container; (B') joining one end of the wound fiber substrate to a substrate fixing element provided in the container; (C) injecting a sol into the container and impregnating the fiber substrate Material; (D) seal the container, defoam the sol by changing the pressure, and gel the sol; (D') rotate the container, the core, or both; and (E) in the container Inject a surface treatment solution into it, and dry the fiber substrate.

Here, the steps (A), (B), (C), (D) and (E) are as described above.

After step (B), one end of the wound fiber substrate is engaged with a substrate fixing member provided in the container (step (B')).

Specifically, one end of the wound fiber substrate is engaged with the substrate fixing device provided in the inner wall of the container, so that it can effectively widen the fiber when the container, the core, or both are rotated The inner layer spacing of the substrate.

Furthermore, after step (D), the container, the core, or both are rotated (step (D')).

In this case, the rotation direction of the core, the container, or both is the same as the winding direction in step (A). In this case, the winding roll can be separated more effectively.

In addition, when the container, the core, or both are rotated, the core can be simultaneously reduced in the direction of the center of the core, or the container can be enlarged in the direction opposite to the center of the core.

The details of shrinking the core in the direction of the center of the core, or enlarging the container in the direction opposite to the center of the core, are the same as described in step (D'').

According to the preparation method described above, an aerogel composite material with excellent thermal conductivity and uniform pore distribution can be produced without using separate wetting steps or separators.

In addition, because all the steps in the method are performed in the container of the apparatus for preparing aerogel composite materials, a high yield of aerogel composite materials can be produced in a simple and economical manner. Aerogel composite

The aerogel composite material according to an embodiment is made using the "method for preparing aerogel composite material" described above. In addition, the aerogel composite material according to an embodiment can be made using the "method for preparing aerogel composite material" described above and using the "device for preparing aerogel composite material" described above .

Therefore, for details of the apparatus for preparing aerogel composite materials and the method for preparing aerogel composite materials, please refer to the above.

The thermal conductivity of the aerogel composite material is 1000 mW/mK or lower, 500 mW/mK or lower, 250 mW/mK or lower or 100 mW/mK or lower, specifically 1 to 50 mW/mK, 5 to 30 mW/ mK, 10 to 25mW/mK, but not limited to this.

If the surface contact angle of the aerogel composite is measured, it can be 95 to 170°, 100 to 160°, 110 to 165°, 110 to 150°, 110 to 130° or 110 to 120°, but not Limited to this.

The density of the aerogel composite material is 0.02 to 0.5 g/cm ³ or 0.03 to 0.3 g/cm ³ . Specifically, the density of the aerogel composite material may be 0.05 to 0.2 g/cm ³ , more specifically 0.1 to 0.15 g/cm ³ , but is not limited thereto.

The porosity of the aerogel composite material is 50 to 99%. Specifically, the porosity of the aerogel composite material may be 70 to 99%, 80 to 99%, and more specifically 90 to 99%, but is not limited thereto.

The inner surface area of the aerogel composite material is 100 to 3,000 cm ² /g. Specifically, the inner surface area of the aerogel composite material may be 200 to 2,500 cm ² /g or 200 to 1,500 cm ² /g, more specifically, 300 to 1,000 cm ² /g, but is not limited thereto. Carrying out examples of embodiments of the present invention

Thereafter, the present invention will be described in detail based on the following examples. However, the following examples are used to further describe the present invention. The scope of the present invention is not limited to this. Example 1

The non-woven fabric (or fibrous substrate) is wound on the core, and then the wound 4-layer roll is inserted into the container of the device for preparing the aerogel composite material. The winding roll is joined to the core fixing element provided at the lower center part of the container of the device for preparing aerogel composite material. After that, a silica-based sol was injected into the container and immersed in the fibrous base material for about 0.5 hours. Seal the container, and then reduce the pressure to 10 Torr for defoaming and gelation for about 0.5 hours. Thereafter, the core is reduced in the center direction of the core. In this case, the cross-sectional area of the reduced core is about 50% of the cross-sectional area of the core before reduction. After that, the fibrous base material is washed with distilled water in an amount of 1.5 to 2 times the weight of the fibrous base material at 70°C for 5 to 25 times, and then the acetone is used in an amount of 1.5 to 2 times the weight of the fibrous base material at 70°C. Stir and wash for three hours with stirring. After that, use 1.5 to 2 times the weight of the fibrous base material IPA at 70 °C with stirring and wash for 3 hours twice, and then use the fibrous base material to the 1.5 to 2 times the amount of hexane at 70 °C Wash with stirring for 3 hours. Subsequently, it was stirred for 3 hours at 50°C in a mixed solution with a hexane to TMCS ratio of 3:1 and an amount 1.5 to 2 times the weight of the fiber substrate. After 12 hours, stir at 70°C for 4 hours. After that, the fibrous base material is cooled to room temperature, simply washed with hexane in an amount of 1.5 to 2 times the weight of the fibrous base material, and then dried. Specifically, after drying at 50°C for 1 hour, drying at 110°C for 3 hours. Evaluation example 1 : Surface photos

FIG. 6 shows the observation results of the surface of the fibrous base material after injecting the sol into the container and impregnating the sol into the fibrous base material and reducing the pressure of the container for defoaming and gelation in Example 1. FIG. As shown in FIG. 6, when the fibrous substrate is layered, the surfaces of the fibrous substrate after gelation can be easily separated from each other, and the surface is not damaged during the layering.

In addition, FIG. 7 shows the observation results of the surface of the fibrous base material after gelation, shrinkage of the core, surface treatment, and drying. As can be seen in FIG. 7, the surface of the fiber substrate is not damaged, and there is no phenomenon of powder falling from it. Evaluation example 2 : Internal photos

8 and 9 are SEM photographs showing the inside of the fiber substrate of the second layer in the four-layer wound roll of the aerogel composite material prepared in Example 1. FIG. Specifically, FIG. 8 is a SEM photograph at 50,000 times magnification inside the aerogel composite, and FIG. 9 is a SEM photograph at 10,000 magnification inside the aerogel composite. It can be seen from Figs. 8 and 9 that the network and pores of the aerogel are stably formed. Evaluation example 3 : Confirmation of surface hydrophobicity

10 and 11 show the results of confirming the surface hydrophobicity of the aerogel composite material prepared in Example 1. Specifically, Phoenix 300 (SEO, Korea) was used to measure the surface contact angle of a part of the surface of the fiber substrate of the second layer of the four-layer wound roll of the aerogel composite material prepared in Example 1. As shown in the results shown in FIGS. 10 and 11, the surface contact angles are 157.35° (FIG. 10) and 157.89° (FIG. 11). This means that the surface is hydrophobic, because the network and pores of the aerogel thus produced are stably formed. Evaluation Example 4 : Thermal conductivity

The thermal conductivity of the aerogel composite prepared in Example 1 was measured according to ASTM C 518, ISO 8301, JIS A 1412, and Laser Comp Corp. (USA) KS L 9106 and Fox 200. Therefore, the measured thermal conductivity is about 20mW/mK.

From the results of Evaluation Examples 1 to 4, it was confirmed that the method for preparing an aerogel composite material according to this embodiment can easily produce a low thermal conductivity and improvement without a separate wetting step and a separator Aerogel composite material with thermal insulation properties.

1‧‧‧Container 2‧‧‧Core fixing element 3‧‧‧Core 4‧‧‧Fiber base material 11, 12, 13‧‧‧ Device a1‧‧‧Core reduces the diameter of the front core a2‧‧ ‧Diameter of core after reduction of core b1‧‧‧Diameter of container before expansion of container b2 ‧‧‧Diameter of container after expansion of container 101a, 101b ‧‧‧Fixed core member 102a, 102b ‧‧‧ Multiple fragments 103a ,103b‧‧‧Fixed container wall 104a,104b‧‧‧Multiple fragments 105a‧‧‧Area with a circle of diameter b1 105b‧‧‧Area of a circle with diameter b2

FIG. 1 depicts an apparatus for preparing an aerogel composite material before and after reduction of a core according to an embodiment. Figure 2 depicts an apparatus for preparing aerogel composites before and after expansion of a container according to an embodiment. 3 is a cross-sectional view of the core body according to this embodiment before and after reduction of the core body. Fig. 4 is a cross-sectional view of an enlarged front and rear container according to this embodiment. Fig. 5 depicts an example of a cross section of the container/core according to this embodiment when it is reduced and enlarged. FIG. 6 depicts the observation results of the surface of the fiber substrate after gelation during the preparation of the aerogel composite. Figure 7 depicts the observation results of the surface of the fibrous substrate after drying during the preparation of the aerogel composite. 8 and 9 are SEM photographs in the aerogel composite material according to the embodiment. 10 and 11 describe the confirmation results of the hydrophobicity of the surface of the aerogel composite material according to the examples. DESCRIPTION OF SYMBOLS 1...Container 2...Core fixing element 3...Core 4...Fiber base material 11...Core reduction and container expansion device for preparing aerogel composite material 12...Core reduction after use Apparatus 13 for preparing aerogel composite material... Apparatus for preparing aerogel composite material after container expansion a1... core body diameter before core reduction a2... core body diameter after core reduction b1... container before expansion container The diameter b2... the diameter 101a of the container after the expansion of the container... the fixed core member 102a before the core is reduced... the plurality of fragments 101b spaced before the core is reduced... the fixed core member 102b after the core is reduced... the core A plurality of fragments 103a after the body is reduced... a fixed container wall 104a before the container is expanded... a plurality of fragments 105a spaced apart before the container is expanded... a cross-sectional area 103b inside the container before the container is expanded... a fixed container wall 104b after the container is expanded... The multiple fragments 105b after the expansion of the container...the cross-sectional area of the interior of the container after the expansion of the container

1‧‧‧Container

2‧‧‧Core fixing element

3‧‧‧Core

4‧‧‧ fiber base material

11, 12‧‧‧ device

a1‧‧‧Core reduces the diameter of the front core

a2‧‧‧The diameter of the core after shrinking

b1‧‧‧The diameter of the container before expansion

Claims (29)

An apparatus for preparing an aerogel composite material includes: a container; a core fixing element provided in the container; and a core, which can be engaged with the core fixing element. The apparatus for preparing an aerogel composite material according to claim 1, wherein the container, the core, or both can be reduced or enlarged. An apparatus for preparing an aerogel composite material according to claim 2, wherein the core body is shrinkable in the center direction of the core body. An apparatus for preparing an aerogel composite material according to claim 2, wherein the container is expandable in the direction opposite to the center of the core. The apparatus for preparing an aerogel composite material according to claim 1, further comprising a substrate fixing member provided in the container. An apparatus for preparing an aerogel composite material according to claim 3, wherein the cross-sectional area of the core body after the core body is reduced is 5 to 90% of the cross-sectional area of the core body before the core body is reduced. An apparatus for preparing an aerogel composite material according to claim 4, wherein after the container is enlarged, the cross-sectional area inside the container is 105 to 150% of the cross-sectional area of the container before the container is enlarged. The device for preparing an aerogel composite material according to claim 1, wherein the container, the core or both are composed of a plurality of fragments, and the container, the core or both may be adjacent to each other as they The multiple fragments are spaced apart or overlapped to shrink or expand. An apparatus for preparing an aerogel composite material according to claim 2, wherein the container, the core, or both are rotatable. An apparatus for preparing an aerogel composite material, comprising: a container; a core fixing element provided in the container; a base material fixing element provided in the container; and a core Can be engaged with the core fixing element, wherein the container, the core or both are rotatable. An apparatus for preparing an aerogel composite material according to claim 10, wherein the container, the core, or both can be reduced or enlarged. An apparatus for preparing an aerogel composite material according to claim 1 or 10, wherein the cross-sectional area of the core is 1 to 40% of the cross-sectional area inside the container. An apparatus for preparing an aerogel composite material according to claim 1 or 10, wherein the core fixing element and the core can be separated from the container, respectively. An apparatus for preparing an aerogel composite material according to claim 1 or 10, wherein the core is vertically fixed to the lower part of the container through the core fixing element. A method for preparing an aerogel composite material, comprising: (A) winding a fiber substrate on a core; (B) placing the core wound with the fiber substrate in a container (C) Inject a sol into the container and impregnate it into the fiber substrate; (D) Seal the container, defoam the sol by changing the pressure, and gel the sol; and (E ) Inject a surface treatment solution into the container and dry the fibrous substrate. The method for preparing an aerogel composite material according to claim 15, wherein step (B) is a step of placing the core wound with the fiber base material in the container and engaging with the core fixing element. The method for preparing an aerogel composite material according to claim 15 further includes: (D'') after step (D), shrinking the core body in the center direction of the core body, or The center of the body expands the container in the opposite direction. The method for preparing an aerogel composite material according to claim 17, wherein after the core body is reduced, the cross-sectional area of the core body is 40 to 95% of the cross-sectional area of the core body before the core body is reduced. The method for preparing an aerogel composite material according to claim 17, wherein after the container is enlarged, the cross-sectional area inside the container is 105 to 150% of the cross-sectional area of the container before the container is enlarged. The method for preparing an aerogel composite material according to claim 17, wherein when the core is reduced, the container, the core, or both can be rotated at the same time. The method for preparing an aerogel composite material according to claim 17, wherein when the container is enlarged, the container, the core, or both can be rotated at the same time. The method for preparing an aerogel composite material according to claim 20 or 21, wherein the rotation direction of the core or the container is the same as the winding direction of step (A). A method for preparing an aerogel composite material, comprising: (A) winding a fiber substrate on a core; (B) placing the core wound with the fiber substrate in a container (B') One end of the wound fiber substrate is engaged with a substrate fixing element provided in the container; (C) A sol is injected into the container and impregnated into the fiber substrate; D) Seal the container, defoam the sol by changing the pressure, and gel the sol; (D') rotate the container, the core or both; and (E) inject a surface into the container Treat the solution and dry the fibrous substrate. The method for preparing an aerogel composite material according to claim 23, wherein step (B) is a step of placing the core wound with the fiber base material in the container and engaging with the core fixing element. The method for preparing an aerogel composite material according to claim 23, wherein the rotation direction of the core or the container is the same as the winding direction of step (A). The method for preparing an aerogel composite material according to claim 23, wherein when the container, the core, or both are rotated, the core is reduced in the center direction of the core at the same time, or may be The center of the body expands the container in the opposite direction. The method for preparing an aerogel composite material according to claim 15 or 23, wherein a single layer to 100 layers of the fibrous substrate are wound on the core. The method for preparing an aerogel composite material according to claim 16 or 24, wherein the core fixing element is placed under the container, and the core system wound with the fibrous base material passes through the core fixing element Fix vertically. An aerogel composite material produced by the method for preparing an aerogel composite material according to claim 15 or 23.

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