KR102037425B1 - Method for preparing aerogel composites and apparatus therefor - Google Patents

Abstract

Examples include a container; A core fixing device provided in the container; And a core capable of being combined with the core fixing device, wherein the container, the core, or both thereof are contractable or expandable, and may provide an airgel composite manufacturing apparatus and a method of manufacturing an airgel composite using the same.

Description

Airgel composite manufacturing method and manufacturing apparatus therefor {METHOD FOR PREPARING AEROGEL COMPOSITES AND APPARATUS THEREFOR}

The embodiment relates to a method for producing an airgel composite without a separator and a manufacturing apparatus therefor.

Aerogels are the lightest solids ever developed by humans and are super insulating materials with a porosity of over 95%. Aerogel is a new material that has been attracting attention as a heat insulating material and a soundproofing material in the future, and recently, research is being conducted to be widely used in various industrial fields. Aerogels generally have a low density, open cell structure, large surface area and nanometer pore size.

Attempts have been made using a belt conveyor impregnation to improve the processability of manufacturing such aerogels (see Korean Patent No. 1133025 and FIG. 1). However, in the conventional belt conveyor impregnation method, an appropriate viscosity is required in order to prevent sol flow loss. A high viscosity sol impregnation may cause bubbles in the aerogel to degrade performance. In order to solve this problem, it is necessary to give sufficient transfer time to reduce bubbles and uniformly impregnate operation, but accordingly, the length of the conveyor belt is increased and additional burrs generated by the roller pressing process are removed. This has a problem of deterioration. In addition, the belt conveyor impregnation method has to be gelated to a level that can be rolled with the reaction during the transfer, but has a limitation that can not give enough gelation time required for the formation of nano-pores that require high quality.

In addition, according to the conventional method, the sol viscosity was lowered and the sol was partially insufficient or not uniform even after the impregnation operation, and the sol was additionally injected from the aging tank to compensate for the insufficient sol. Partial desorption and scattering in powder form pointed out difficulties in construction and resulted in degradation of performance quality.

In addition, when the separation membrane is used to separate the composite after gelling in a roll state, there is a problem in that efficiency is lowered by adding a manufacturing process such as a membrane insertion process before sol impregnation and a membrane removal process before gelation and washing step.

Korean Registered Patent Publication No. 1133025

Example is to use a batch method instead of a continuous method to prepare aerogel-formed composite, using a natural separation method of the fibrous substrate without the use of a membrane, economically to prepare a method and use of the airgel composite To provide a manufacturing apparatus.

Airgel composite manufacturing apparatus according to one embodiment comprises a container; A core fixing device provided in the container; And a core engageable with the core anchor, wherein the vessel, the core, or both are retractable or expandable.

Airgel composite manufacturing apparatus according to another embodiment includes a container; A core fixing device provided in the container; A substrate fixing device provided in the container; And a core engageable with the core fixture, wherein the vessel, the core, or both are rotatable.

Method for producing an airgel composite according to one embodiment comprises the steps of (a1) winding a fibrous substrate in the core; (b1) placing the fibrous substrate wound core in a container and engaging a core fixture; (c1) injecting a sol into the container and impregnating the fibrous substrate; (d1) sealing the vessel, defoaming under reduced pressure and gelling the sol; (e1) contracting the core in the core center direction or expanding the container in the opposite direction of the core center; And (f1) injecting a surface treatment solution into the container and then drying it.

According to another embodiment, a method of manufacturing an airgel composite includes (a2) winding a fibrous substrate on a core; (b2-1) placing the fibrous substrate wound core in a container and engaging the core retainer; (b2-2) combining one end of the wound fibrous substrate with a substrate fixing device provided in the container; (c2) injecting a sol into the container and impregnating the fibrous substrate; (d2) sealing the vessel, defoaming under reduced pressure and gelling the sol; (e2) rotating the vessel, the core or both; And (f2) injecting a surface treatment solution into the container and then drying it.

In addition, the airgel composite is prepared by the method for producing the airgel composite.

According to the airgel composite manufacturing apparatus according to the embodiment and a method for producing an airgel composite using the same, regardless of the viscosity of the sol can be produced an airgel composite having a low thermal conductivity and improved thermal insulation performance without a membrane.

In addition, according to the manufacturing method can shorten the manufacturing process is economical, it is possible to easily mass-produce the airgel composite.

Figure 1 shows the airgel composite manufacturing apparatus before and after core shrinkage according to the embodiment.
Figure 2 shows the airgel composite production apparatus before and after the container expansion according to the embodiment.
3 is a cross-sectional view of a core before and after core shrinkage according to an embodiment.
4 is a cross-sectional view of the vessel before and after vessel expansion according to an embodiment.
5 illustrates an example of a cross section upon contraction and expansion of a container / core in accordance with an embodiment.
6 is a result of observing the surface of the fibrous substrate after gelling during the preparation of the airgel composite.
7 is a result of observing the surface of the fibrous substrate after drying during the preparation of the airgel composite.
8 and 9 are SEM pictures of the interior of the airgel composite according to the embodiment.
10 and 11 are the results confirming the surface hydrophobicity of the airgel composite according to the embodiment.

Hereinafter, the present invention will be described in detail through examples. The embodiments may be modified in various forms unless the gist of the invention is changed.

Criteria for the top and bottom of each component will be described based on the drawings. In addition, the same reference numerals in the drawings refer to the same components, the size or thickness of each component may be exaggerated for convenience of description.

"Including" in the present specification means that it may further include other components unless otherwise specified.

In addition, all numbers and expressions indicating content of components, reaction conditions, and the like, unless otherwise indicated, are to be understood as being modified by the term "about."

< Airgel  Composite Manufacturing Equipment>

Airgel composite manufacturing apparatus according to an embodiment is an apparatus for economically manufacturing the airgel composite using a batch method without a membrane.

Airgel composite manufacturing apparatus (11, 12, 13) according to an embodiment, the container (1); A core fixing device (2) provided inside the container; And a core 3 coupleable with the core fixing device. At this time, the container, the core or both are retractable or expandable (see FIGS. 1 and 2).

Figure 1 shows the device for producing an airgel composite as the core is contracted, Figure 2 shows the device for producing an airgel composite as the container is expanded.

1 and 2, a1 is the diameter of the core before core shrinkage, a2 is the diameter of the core after core shrinkage, b1 is the diameter of the container before container expansion, b2 is the diameter of the container after container expansion, a1 is larger than a2, b1 is less than b2.

The core fixing device 2 and the core 3 are separable from the container 1, respectively.

The material of the container 1 is not particularly limited, but can be used if the material having chemical resistance. Specifically, stainless steel material, coated metal material or glass may be used.

The shape of the container is not particularly limited, but may be cylindrical, considering the shape of the fibrous substrate wound on the core. In addition, the size of the container is not particularly limited, and may be appropriately selected in consideration of the size of the fibrous substrate wound on the core.

The material of the core fixing device 2 is not particularly limited, but can be used if the material having chemical resistance. Specifically, stainless steel material, coated metal material or glass may be used.

The core may be fixed perpendicularly to the lower part of the container through the core fixing device. Specifically, it may be fixed vertically to the lower portion in the container. More specifically, it may be vertically fixed to the lower center in the container, but is not limited thereto.

The core fixing device 2 is rotatable. Specifically, the core fixing device may rotate about the longitudinal center axis of the core when the core is fixed.

The material of the core 3 is not particularly limited, but any material having chemical resistance may be used. Specifically, stainless steel material, coated metal material, glass, plastic or compressed pulp may be used.

The core may have a cylindrical shape, but is not limited thereto.

The container, the core or both comprise a plurality of pieces. Or the container, the core or both may be of a plurality of pieces.

Adjacent pieces of the plurality of pieces adjacent to each other are spaced apart or overlapping, the container, the core or both can shrink or expand.

Alternatively, the container, the core, or both of the plurality of pieces may be contracted or expanded by being spaced apart or abutting each other.

Alternatively, the container, the core, or both may be contracted or expanded by abutting or overlapping adjacent pieces of the plurality of pieces.

The core can shrink in the core center direction.

In detail, the core may include a core fixing portion 101a and 101b and a plurality of pieces 102a and 102b surrounding the core fixing portion. At this time, the plurality of pieces 102a may be spaced apart from each other with respect to the fixing part, and the plurality of neighboring pieces 102b may be brought into contact with or overlapping with each other, thereby causing the core to contract (see FIG. 3).

In addition, the core may be composed of a plurality of pieces. In this case, the plurality of pieces may be spaced apart from each other, and the plurality of neighboring pieces may come into contact with each other, or the core may shrink. Alternatively, the plurality of pieces may be in contact with each other and then overlap each other to shrink the core (see FIG. 5).

As another example, the core may be in the form of a take-up roll, and may shrink or expand as the gap between the wound materials is adjusted.

As another example, the core may include a core holder and a separator surrounding the core holder, and may be shrunk by removing the separator.

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

The cross sectional area of the core means a cross sectional area orthogonal to the longitudinal direction of the core.

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

The cross sectional area of the core is 1 to 40% of the internal cross sectional area of the vessel. 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 is also expandable in the opposite direction of the core center. In other words, the core is both economical as it can be retracted or expanded to allow reuse of the device.

The vessel is expandable in the opposite direction of the core center.

Specifically, the container may be made of a container fixing wall 103a, 103b and a plurality of pieces 104a, 104b. In this case, the plurality of pieces 104a may be in contact with each other, and the plurality of neighboring pieces 104b may be spaced apart from each other to expand the container (see FIG. 4).

In addition, the container may consist of a plurality of pieces. At this time, the plurality of pieces overlap each other and the container can be expanded while being in contact with each other (see Figure 5).

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

As another example, the container may include a container fixing wall and a separating wall, and the inside of the container may be expanded by removing the separating wall.

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

The cross-sectional area inside the vessel refers to the area of the inner circumference of the bottom of the vessel.

For example, referring to FIG. 4, the cross-sectional area inside the container before the expansion of the container means the area 105a of the circle whose diameter is b1, and the cross-sectional area inside the container after the expansion of the container is a circle of diameter b2. It means the area 105b. b2 is greater than b1.

The container is also capable of shrinking in the core center direction. In other words, the container is economical because it can be retracted or expanded and the device can be reused.

The vessel, the core or both are rotatable.

The core may rotate about a longitudinal central axis of the core. In addition, the container may rotate about the central axis of the container.

The core can rotate about the longitudinal central axis of the core while the vessel, the core or both contract or expand. In addition, the container, the core or both can shrink or expand while at the same time the container can rotate about the central axis of the container.

The airgel composite manufacturing apparatus may further include a substrate fixing device provided inside the container. At this time, the substrate fixing device serves to fix one end of the fibrous substrate.

Airgel composite manufacturing apparatus according to another embodiment, the container; A core fixing device provided in the container; A substrate fixing device provided in the container; And a core coupled to the core fixing device. At this time, the container, the core or both are rotatable.

In the case of the aerogel composite production device wherein the container, the core or both are rotatable, includes a substrate holder.

The substrate fixing device may be provided inside the container. Specifically, the substrate fixing device may be provided on the inner wall of the container. This serves to fix one end of the fibrous substrate.

The airgel composite manufacturing apparatus is the container, the core or both are shrinkable or expandable. Specifically, the core can be contracted in the core center direction and can be expanded for reuse. In addition, the container is expandable in the opposite direction of the core center, and also retractable for reuse.

For the description of the container, the core fixing device, the core and the like, refer to the above description.

The airgel composite manufacturing apparatus is reusable and does not go through unnecessary processes, so the airgel composite manufacturing process is more economical.

< Airgel  Manufacturing Method of Composite>

According to one or more embodiments, a method of manufacturing an airgel composite includes (a1) winding a fibrous substrate on a core; (b1) placing the fibrous substrate wound core in a container and engaging a core fixture; (c1) injecting a sol into the container and impregnating the fibrous substrate; (d1) sealing the vessel, defoaming under reduced pressure and gelling the sol; (e1) contracting the core in the core center direction or expanding the container in the opposite direction of the core center; And (f1) injecting a surface treatment solution into the container and then drying it.

Referring to FIGS. 1 and 2, a method of manufacturing an airgel composite according to an embodiment is as follows.

Airgel composite manufacturing method according to an embodiment uses the above-described 'airgel composite manufacturing apparatus'. Therefore, the contents related to the airgel composite production apparatus, that is, the container, the core fixing device, the core, and the like, refer to the contents described in the above <airgel composite production apparatus>.

First, a fibrous substrate is wound around a core ((a1) step).

The fibrous substrate may be in the form of an elongate mat. For example, the fibrous substrate may be a woven mat or a nonwoven mat, but is not limited thereto.

In addition, the fibrous substrate 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 fibers, glass wool, rock wool, ceramic wool, and boron fibers, but It is not limited.

The organic fiber may be nylon, aramid fiber, carbon fiber, polypropylene fiber, polyethylene fiber, polyester fiber, polyurethane fiber, acrylic fiber, polyvinyl chloride acetate fiber, rayon fibers, rayon fibers, regenerated fibers, And waste fibers (waste fibers) may be one or more selected from the group consisting of, but is not limited thereto, and other special fibers or general fibers such as cotton (cotton) or linn (linen) used in life is also possible.

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

The fibrous substrate may be wound in a core of 1 ply to 100 ply, but is not limited thereto. Specifically, the fibrous substrate may be wound in two to fifty layers on the core. It is preferable to wind suitably according to the thickness of a fibrous base material, and the size of a container.

Next, the core in which the fibrous substrate is wound is placed in the container and combined with the core fixing device (step (b1)).

The core holder 2 is disposed below the container, and the cores 3 and 4 on which the fibrous substrate is wound are vertically fixed through the core holder.

It is economical in that it uses a core wound directly on the fibrous substrate without a separate wetting pretreatment.

Subsequently, a sol is injected into the container and impregnated into the fibrous substrate (step (c1)).

The sol may be one or more selected from the group consisting of zirconia, yttrium oxide, hafnia, alumina, titania, ceria, silica, magnesium oxide, calcium oxide, magnesium fluoride and calcium fluoride.

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

The fibrous substrate is also impregnated for 10 minutes to 2 hours. Specifically, the fibrous substrate may be impregnated for 10 minutes to 1 hour.

Next, the container is sealed and degassed under reduced pressure and the sol is gelled (d1).

The vessel may be sealed and the pressure in the vessel may be reduced to a range of 0.001 to 300 Torr, 0.001 to 100 Torr, or 0.001 to 10 Torr on an absolute pressure basis.

By sealing the vessel and depressurizing it, it is possible to effectively remove bubbles generated by the surface tension of the inorganic or organic fibers when the sol is impregnated into the fibrous material.

Sealing the vessel is in addition to the purpose of reducing the pressure, but also to prevent the collapse of the gel tissue due to drying of the contents in the vessel.

In addition, the defoaming time can be defoamed for 10 minutes to 2 hours. Specifically, it may be defoamed for 10 minutes to 1 hour.

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

Thereafter, the core is contracted in the core center direction, or the container is expanded in the direction opposite to the core center (step (e1)).

The core may be shrunk in the core center direction as described in the airgel composite manufacturing apparatus.

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

The cross sectional area of the core means a cross sectional area orthogonal to the longitudinal direction of the core.

Alternatively, the container may extend in the opposite direction of the core center as described in the airgel composite manufacturing apparatus.

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

At the same time, while retracting the core, the container, the core or both can be rotated. At this time, the rotation direction of the container, the core or the container is the same as the winding direction in the step (a1). In this case, it is more efficient to separate the rolled up roll.

Alternatively, the vessel, the core or both may be rotated at the same time as the vessel is expanded. At this time, the rotation direction of the container, the core or the container is the same as the winding direction in the step (a1). In this case, it is more efficient to separate the rolled up roll.

By shrinking the core in the core direction or expanding the container in the opposite direction of the core center, the volume of the space in which the fibrous substrate wound around the core is present increases, thereby additionally winding the fibrous substrate as the fiber is further wound. The interlayer spacing between the substrates is widened. Increasing the interlayer spacing allows efficient solvent cleaning and surface treatment, and allows the material filled in the pores inside the gel to be effectively replaced by other solvents.

Next, the surface treatment solution is injected into the container and dried (step (f1)).

The surface treatment solution is distilled water; C ₁ -C ₈ alcohols such as isopropyl alcohol; Ketones such as acetone; C ₁ -C ₁₂ alkanes such as hexane; Aromatic solvents such as toluene, xylene and the like; Silane compounds such as trimethylchlorosilane (TMCS), hexamethyldisilazane (HMDS), dimethylchlorosilane (DMCS) and methyltrichlorosilane (MTCS); It is 1 or more types chosen from the group which consists of these.

Specifically, the surface treatment solution may be distilled water, acetone, isopropyl alcohol, hexane, TMCS and the like, but is not limited thereto.

The fibrous substrate may be washed 1 to 50 times at 20 to 80 ° C using the surface treatment solution.

The drying step may be atmospheric pressure drying or supercritical drying.

The atmospheric drying is 60 to 600 minutes at 5 to 350 ℃; Or from 60 to 240 minutes at 20 to 250 ° C.

In addition, the supercritical drying is not particularly limited, but may be performed under conditions of about 100 to 200 atmospheres.

According to another embodiment of the present invention, a method of manufacturing an airgel composite includes (a2) winding a fibrous substrate on a core; (b2-1) placing the fibrous substrate wound core in a container and engaging the core retainer; (b2-2) combining one end of the wound fibrous substrate with a substrate fixing device provided in the container; (c2) injecting a sol into the container and impregnating the fibrous substrate; (d2) sealing the vessel, defoaming under reduced pressure and gelling the sol; (e2) rotating the vessel, the core or both; And (f2) injecting a surface treatment solution into the container and then drying it.

Here, the descriptions of the steps (a2), (b2-1), (c2), (d2) and (f1) are described in the steps (a1), (b1), (c1), Reference is made to the description of steps (d1) and (f2).

After the step (b2-1), one end of the wound fibrous substrate is combined with the substrate fixing device provided in the container (step (b2-2)).

Specifically, by combining one end of the wound fibrous substrate with a substrate holder provided on the inner wall of the container, it is possible to effectively widen the interlayer spacing of the fibrous substrate when rotating the container, the core or both. have.

Also, after the step (d2), the container, the core or both are rotated (step (e2)).

At this time, the rotation direction of the container, the core or the container is the same as the winding direction in the step (a2). In this case, it is more efficient to separate the rolled up roll.

It is also possible to retract the core in the direction of the core center or to expand the container in the opposite direction of the core center while simultaneously rotating the vessel, the core or both.

For the description of shrinking the core in the core center direction or expanding the container in the opposite direction of the core center, refer to that described in step (e1).

According to the above-described manufacturing method, an airgel composite having excellent thermal conductivity and uniform pore distribution can be produced without using a separate wetting process or a separation membrane.

In addition, since all the processes are made in the container of the airgel composite production apparatus, it is possible to produce the airgel composite with high productivity and simple yet economical.

< Airgel  Complex>

The airgel composite according to one embodiment is prepared by the above-described 'method of preparing the airgel composite'. In addition, the airgel composite according to one embodiment may be prepared by the above-described 'method of preparing an airgel composite' using the 'aerogel composite manufacturing apparatus'.

Therefore, the contents related to the airgel composite production apparatus and the airgel composite manufacturing method refer to the above contents.

The thermal conductivity of the airgel composite is 1000 mW / mK or less, 500 mW / mK or less, 250 mW / mK or less, 100 mW / mK or less, specifically 1 to 50 mW / mK, 5 to 30 mW / mK, 10 to It may be 25 mW / mK, but is not limited thereto.

When the surface contact angle of the airgel composite is measured, it may be 95 to 170 °, 100 to 160 °, 110 to 165 °, 110 to 150 °, 110 to 130 ° or 110 to 120 °, but is not limited thereto.

The airgel composite has a density of 0.02 to 0.5 g / cm ³ or 0.03 to 0.3 g / cm ³ . Specifically, the density of the airgel composite 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 airgel composite is 50 to 99%. Specifically, the porosity of the airgel composite may be 70 to 99%, 80 to 99%, more specifically 90 to 99%, but is not limited thereto.

The inner surface area of the airgel composite is 100 to 3,000 cm ² / g. Specifically, the inner surface area of the airgel composite may be 200 to 2500 cm ² / g or 200 to 1500 cm ² / g, more specifically 300 to 1,000 cm ² / g, but is not limited thereto.

[ Example ]

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are only for illustrating the present invention, and the scope of the present invention is not limited thereto.

Example  One

A nonwoven fabric (fibrous substrate) was wound around the core, and a roll wound in four layers was inserted into a container of an airgel composite production apparatus. The rolled roll was bonded to a core fixture disposed at the bottom center in the airgel composite production vessel. A silica based sol was then injected into the vessel and the fibrous substrate was impregnated for about 0.5 hours. The vessel was sealed and reduced in pressure to 10 Torr, then defoamed and gelated for about 0.5 hours. Thereafter, the core was contracted toward the center of the core. At this time, the cross-sectional area of the shrinked core was about 50% of the cross-sectional area before shrinking of the core. Subsequently, it was washed 5 to 25 times at 70 ° C. with distilled water 1.5 to 2 times the weight of the fibrous substrate, followed by 3 times stirring at 70 ° C. for 3 hours at 1.5 to 2 times the amount of acetone of the weight of the fibrous substrate. . After washing twice with stirring at 70 ° C. for 3 hours with 1.5 to 2 times the IPA weight of the fibrous substrate weight, and then stirring at 70 ° C. for 3 hours with 1.5 to 2 times the hexane weight of the fibrous substrate weight. Washed. Subsequently, the solution which mixed 1.5-2 times of hexane: TMCS of the weight of a fibrous base material at 3: 1 was stirred at 50 degreeC for 3 hours, and after 12 hours, it was stirred at 70 degreeC for 4 hours. Thereafter, the mixture was cooled to room temperature, washed briefly with 1.5 to 2 times the weight of hexane of the fibrous substrate, and dried. Specifically, after drying for 1 hour at 50 ℃, it was dried for 3 hours at 110 ℃.

Evaluation example  1: surface photo

In Example 1, a sol was injected into a container, impregnated into the fibrous substrate, degassed under reduced pressure, and gelled, and the result of observing the surface of the fibrous substrate is shown in FIG. 6. As can be seen in Figure 6, after the gelation of the fibrous substrate peeling can be easily separated between the surface, it was confirmed that there is no damage to the surface when peeling the surface.

In addition, the result of observing the surface of the fibrous substrate shrinkage, surface treatment and dried after gelation is shown in Figure 7. As can be seen in Figure 7, it was confirmed that the surface of the fibrous substrate is not damaged and there is no phenomenon that the powder falls.

Evaluation example  2: internal photo

SEM photographs of the insides of the fibrous substrates positioned on two layers of the four-ply rolls of the airgel composite prepared in Example 1 are shown in FIGS. 8 and 9. Specifically, FIG. 8 is a SEM photograph of the inside of the airgel composite at 50,000 magnification, and FIG. 9 is a SEM photograph of the inside of the airgel composite at 10,000 magnification. As can be seen in Figures 8 and 9, it was confirmed that the network and pores of the airgel was formed stably.

Evaluation example  3: confirm surface hydrophobicity

Results of confirming the surface hydrophobization of the airgel composite prepared in Example 1 are shown in FIGS. 10 and 11. Specifically, the surface contact angle of the part of the surface of the fibrous substrate located on two ply of the four-ply roll of the airgel composite prepared in Example 1 was measured using a Phoenix 300 (SEO, Korea) measuring instrument. As a result, as can be seen in Figures 10 and 11, it was confirmed that the surface contact angle is 157.35 ° (Fig. 10), 157.89 ° (Fig. 11). This is a result indicating that the network and pores of the prepared airgel is formed stably to hydrophobize the surface.

Evaluation example  4: thermal conductivity

The thermal conductivity of the airgel composite prepared in Example 1 was measured by Fox200 of Laser comp corp. (USA) based on ASTM C 518, ISO 8301, JIS A 1412, KS L 9106. The thermal conductivity measured at this time was about 20 mW / mK.

It was confirmed through the results of the evaluation examples 1 to 4 that the airgel composite having a low thermal conductivity and an improved thermal insulation performance can be easily produced by the method of preparing the airgel composite according to the embodiment without a separate wetting step and a separator. .

1: container
2: core fixture
3: core
4: fibrous substrate
11: Airgel composite manufacturing device before core shrinkage and container expansion
12: airgel composite manufacturing apparatus after core shrinkage
13: Airgel composite manufacturing apparatus after container expansion
a1: diameter of core before core shrink
a2: diameter of core after core shrink
b1: diameter of the container before container expansion
b2: diameter of the container after container expansion
101a: core fixing before core shrink
102a: Multiple pieces spaced before core shrinkage
101b: core fixture after core shrinkage
102b: Multiple pieces after core shrink
103a: container holding wall before container expansion
104a: Multiple pieces before container expansion
105a: Cross section inside the vessel before expansion
103b: container holding wall after container expansion
104b: Multiple pieces after container expansion
105b: cross-sectional area inside the vessel after vessel expansion

Claims (25)

Vessel;
A core fixing device provided in the container; And
Includes a core that can be coupled to the core fixing device,
Apparatus for producing an airgel composite, wherein said container, said core or both are shrinkable or expandable.
The method of claim 1,
The core is shrinkable in the core center direction, airgel composite manufacturing apparatus.
The method of claim 1,
Air vessel composite manufacturing apparatus, the container is expandable in the opposite direction of the core center.
The method of claim 1,
The substrate fixing device provided inside the container; further comprising, airgel composite manufacturing apparatus.
The method of claim 2,
And the cross-sectional area of the core after the core shrinks is 5 to 90% of the cross-sectional area of the core before the core shrinks.
The method of claim 3,
And wherein the cross-sectional area inside the container after the container is expanded is 105 to 150% of the cross-sectional area of the container before the container is expanded.
The method of claim 1,
The container, the core or both consisting of a plurality of pieces,
Adjacent pieces of the plurality of pieces adjacent to each other spaced apart or overlapping, or expandable, airgel composite manufacturing apparatus.
The method of claim 1,
Apparatus for producing an airgel composite, wherein the vessel, the core or both are rotatable.
Vessel;
A core fixing device provided in the container;
A substrate fixing device provided in the container; And
Includes a core that can be coupled to the core fixing device,
Apparatus for producing an airgel composite, wherein the vessel, the core or both are rotatable.
The method of claim 9,
Apparatus for producing an airgel composite, wherein said container, said core or both are shrinkable or expandable.
The method according to claim 1 or 9,
Apparatus for producing an airgel composite, wherein the cross-sectional area of the core is 1 to 40% of the internal cross-sectional area of the container.
The method according to claim 1 or 9,
The core fixing device and the core are each separated from the container, the airgel composite manufacturing apparatus.
The method according to claim 1 or 9,
Apparatus for producing an airgel composite, wherein the core is fixed vertically to the bottom in the container through the core fixing device.
(a1) winding the fibrous substrate to the core;
(b1) placing the fibrous substrate wound core in a container and engaging a core fixture;
(c1) injecting a sol into the container and impregnating the fibrous substrate;
(d1) sealing the vessel, defoaming under reduced pressure and gelling the sol;
(e1) contracting the core in the core center direction or expanding the container in the opposite direction of the core center; And
(f1) injecting a surface treatment solution into the container and drying it.
The method of claim 14,
In the step (e1),
And a cross-sectional area of the core after shrinking the core is 40 to 95% of the cross-sectional area of the core before shrinking the core.
The method of claim 14,
In the step (e1),
And wherein the cross-sectional area inside the vessel after expanding the vessel is 105 to 150% of the cross-sectional area of the vessel before the vessel expands.
The method of claim 14,
In the step (e1),
Simultaneously rotating the vessel, the core or both while shrinking the core.
The method of claim 14,
In the step (e1),
Simultaneously rotating the vessel, the core or both while expanding the vessel.
The method of claim 17 or 18,
The direction of rotation of the core or the container is the same as the winding direction in the step (a1), a method for producing an airgel composite.
(a2) winding the fibrous substrate to the core;
(b2-1) placing the fibrous substrate wound core in a container and engaging the core retainer;
(b2-2) combining one end of the wound fibrous substrate with a substrate fixing device provided in the container;
(c2) injecting a sol into the container and impregnating the fibrous substrate;
(d2) sealing the vessel, defoaming under reduced pressure and gelling the sol;
(e2) rotating the vessel, the core or both; And
(f2) injecting a surface treatment solution into the container and drying it.
The method of claim 20,
In the step (e2),
The rotation direction of the core or the container is the same as the winding direction in the step (a2), the method of manufacturing an airgel composite.
The method of claim 20,
In the step (e2),
Simultaneously rotating the vessel, the core or both while shrinking the core in the core direction or extending the vessel in the opposite direction of the core center.
The method of claim 14 or 20,
A method for producing an airgel composite, wherein the fibrous substrate is wound on a core in 1 to 100 layers.
The method of claim 14 or 20,
Disposing the core holder under the container and vertically fixing the core on which the fibrous substrate is wound through the core holder.
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