Method for manufacturing a plurality of bodies made of a porous material
20220289928 · 2022-09-15
Assignee
Inventors
- Dirk Weinrich (Lemfoerde, DE)
- Volker Vogelsang (Lemfoerde, DE)
- Rene Thomas Wiegmann (Lemfoerde, DE)
- Sohaji Movahhed (Koeln, DE)
- Marc Fricke (Lemfoerde, DE)
- Torben Kaminsky (Lemfoerde, DE)
- Maria Thomas (Lemfoerde, DE)
- Joerg Erbes (Ludwigshafen, DE)
- Wibke Loelsberg (Ludwigshafen am Rhein, DE)
Cpc classification
C08G18/7671
CHEMISTRY; METALLURGY
Y02A30/242
GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
C08J2205/026
CHEMISTRY; METALLURGY
C08J9/286
CHEMISTRY; METALLURGY
B01J20/28045
PERFORMING OPERATIONS; TRANSPORTING
C08J2205/02
CHEMISTRY; METALLURGY
C08J2201/05
CHEMISTRY; METALLURGY
International classification
C08J9/28
CHEMISTRY; METALLURGY
Abstract
A method can be used for manufacturing one or more bodies made of a porous material derived from precursors of the porous material in a sol-gel process. The method involves filling precursors of the porous material into a mold defining the shape of the body, where the precursors include at least two reactive components and a solvent, and forming a gel body. The step is then repeated so as to form several gel bodies. The gel bodies are then removed from the mold after a predetermined time in which the gel bodies are formed from the precursors of the porous material. The gel bodies are arranged adjacent to one another, a spacer is provided between two adjacent gel bodies so as to provide a clearance therebetween, and the solvent is then removed from the gel bodies.
Claims
1: A method for manufacturing a plurality of bodies made of a porous material derived from precursors of the porous material in a sol-gel process, the method comprising: (i) filling precursors of a porous material into a mold defining a shape of a body, wherein the precursors include at least two reactive components and a solvent, and forming a gel body, (ii) repeating (i) so as to form a plurality of gel bodies, (iii) removing the plurality of gel bodies from the mold after a predetermined time in which the plurality of gel bodies are formed from the precursors of the porous material, (iv) arranging the plurality of gel bodies adjacent to one another, (v) providing a spacer between two adjacent gel bodies so as to provide a clearance therebetween, and (vi) removing the solvent from the plurality of gel bodies.
2: The method according to claim 1, wherein the spacer is a grid assembly comprising a first grid and a second grid connected to one another, wherein the first grid comprises first openings and the second grid comprises second openings, wherein the first openings and the second openings are shifted relative to one another.
3: The method according to claim 2, wherein the grid assembly comprises a thickness of 1.0 mm to 4.0 mm, and/or wherein the first openings and/or the second openings are arranged in a regular or irregular pattern, and/or wherein the first openings and/or the second openings comprise identical or different opening areas, and/or wherein the first openings and/or the second openings comprise identical or different shapes, and/or wherein the first openings and/or the second openings comprise a circular, oval, elliptical, polygonal, polygonal including rounded edges, rectangular, or square shape, and/or wherein the method further comprises at least partially providing surfaces of the first grid and/or the second grid with a coating made of a material being electrically dissipative and non-sticky to the plurality of gel bodies, and/or wherein a total opening area of the first openings and the second openings is 40% to 95% of a facing outer surface of one of the plurality of gel bodies.
4: The method according to claim 1, further comprising integrally forming each of the plurality of gel bodies with the spacer.
5: The method according to claim 4, wherein the spacer includes a plurality of protrusions protruding from at least one surface of the plurality of gel bodies.
6: The method according to claim 5, further comprising forming the plurality of protrusions only on one of the at least one surface of each of the plurality of gel bodies, wherein the plurality of gel bodies are arranged adjacent to one another such that the at least one surface including the plurality of protrusions of one of the plurality of gel bodies faces a surface without protrusions of a respective adjacent gel body.
7: The method according to claim 5, wherein each of the plurality of protrusions comprises a circular cross-sectional shape with a diameter of 1.0 to 5.0 mm, and/or wherein the plurality of protrusions are arranged in a regular or irregular pattern, and/or wherein the plurality of protrusions have identical or different shapes, and/or wherein the plurality of protrusions have a height of 0.1 mm to 20.0 mm, and/or wherein the plurality of protrusions are arranged such that a minimum distance between outer surfaces of adjacent protrusions is 0.1 mm, and/or wherein the plurality of protrusions are formed as truncated cones, and/or wherein the method further comprises removing the plurality of protrusions after removing the solvent from the plurality of gel bodies.
8: The method according to claim 1, wherein the plurality of gel bodies are formed as slabs having a cuboid, cylindrical, or polygonal shape, and wherein the plurality of gel bodies are arranged such that side surfaces of the cuboid, cylindrical, or polygonal shape having a greatest surface area are oriented substantially perpendicular with respect to a direction of gravity, or wherein the plurality of gel bodies are arranged such that side surfaces of the cuboid, cylindrical, or polygonal shape having the greatest surface area are oriented substantially parallel with respect to a direction of gravity.
9: The method according to claim 1, wherein the plurality of gel bodies are formed as slabs comprising a length of at least 10 cm and a width of at least 10 cm, and/or wherein the plurality of gel bodies are formed as slabs comprising a thickness of at least 0.5 mm.
10: The method according to claim 1, wherein the spacer is a grid comprising grid openings.
11: The method according to claim 10, wherein the grid openings comprise identical or different opening areas, and/or wherein the grid openings are arranged in a regular or irregular pattern, and/or wherein the grid comprises struts defining the grid openings, wherein the struts comprise a width of 1.0 mm to 5.0 mm, and/or wherein the plurality of gel bodies are formed as slabs having a cuboid, cylindrical, or polygonal shape, wherein the plurality of gel bodies are arranged such that side surfaces of the cuboid, cylindrical, or polygonal shape having a greatest surface area are oriented substantially perpendicular with respect to a direction of gravity, and/or wherein the method further comprises at least partially providing surfaces of the grid with a coating made of a material being electrically dissipative and non-sticky to the plurality of gel bodies.
12: The method according to claim 10, wherein removing the solvent from the plurality of gel bodies is performed by means of supercritical drying.
13: The method according to claim 10, wherein the grid is configured to carry each of the plurality of gel bodies and to support a second grid disposed thereon without the plurality of gel bodies being engaged by the second grid.
14: The method according to claim 1, wherein removing the solvent from the plurality of gel bodies is performed by means of supercritical drying or convective drying.
15: A plurality of gel bodies obtained or obtainable by the process according to claim 1.
16: A thermal insulation material or a vacuum insulation panel, comprising the plurality of gel bodies according to claim 15.
17: A method, comprising: molding a thermal insulation material or a vacuum insulation panel comprising the plurality of gel bodies according to claim 15.
18: The method according to claim 3, wherein the grid assembly comprises a thickness of 1.5 mm to 2.5 mm.
19: The method according to claim 4, wherein the forming comprises monolithically forming each of the plurality of gel bodies with the spacer.
20: The method according to claim 13, wherein the grid comprises an outer rim configured to support the second grid disposed thereon, without the plurality of gel bodies being engaged by the second grid.
Description
SHORT DESCRIPTION OF THE FIGURES
[0216] Further features and embodiments of the invention will be disclosed in more detail in the subsequent description, particularly in conjunction with the dependent claims. Therein the respective features may be realized in an isolated fashion as well as in any arbitrary feasible combination, as a skilled person will realize. The embodiments are schematically depicted in the figures. Therein, identical reference numbers in these figures refer to identical elements or functionally identical elements.
[0217] In the Figures:
[0218]
[0219]
[0220]
[0221]
[0222]
[0223]
[0224]
[0225]
DETAILED DESCRIPTION
[0226] As used in the following, the terms “have”, “comprise” or “include” or any arbitrary grammatical variations thereof are used in a non-exclusive way. Thus, these terms may both refer to a situation in which, besides the feature introduced by these terms, no further features are present in the entity described in this context and to a situation in which one or more further features are present. As an example, the expressions “A has B”, “A comprises B” and “A includes B” may both refer to a situation in which, besides B, no other element is present in A (i.e. a situation in which A solely and exclusively consists of B) and to a situation in which, besides B, one or more further elements are present in entity A, such as element C, elements C and D or even further elements.
[0227] Further, it shall be noted that the terms “at least one”, “one or more” or similar expressions indicating that a feature or element may be present once or more than once typically will be used only once when introducing the respective feature or element. In the following, in most cases, when referring to the respective feature or element, the expressions “at least one” or “one or more” will not be repeated, non-withstanding the fact that the respective feature or element may be present once or more than once.
[0228] Further, as used in the following, the terms “particularly”, “more particularly”, “specifically”, “more specifically” or similar terms are used in conjunction with additional/alternative features, without restricting alternative possibilities. Thus, features introduced by these terms are additional/alternative features and are not intended to restrict the scope of the claims in any way. The invention may, as the skilled person will recognize, be performed by using alternative features. Similarly, features introduced by “in an embodiment of the invention” or similar expressions are intended to be additional/alternative features, without any restriction regarding alternative embodiments of the invention, without any restrictions regarding the scope of the invention and without any restriction regarding the possibility of combining the features introduced in such way with other additional/alternative or non-additional/alternative features of the invention.
[0229] Further, it shall be noted that the terms “first”, “second” and “third” are used to exclusively facilitate to differ between the respective constructional members or elements and shall not be construed to define a certain order or importance.
[0230] The term “mold” as used herein refers to a hollowed-out block or container that is configured to be filled with a liquid or pliable material provided by precursors of a sol gel provided by precursors of a sol gel. Particularly, the sol-gel process is carried out within the mold. During the sol-gel process the precursors form a sol which subsequently starts to gel. Thus, the liquid hardens or sets inside the mold, adopting its shape defined by the interior volume thereof. The mold is basically used to carry out the sol-gel process. However, it is to be noted that the solvent may be removed from the thus formed gel with the gel remaining within the mold or with the gel removed from the mold. In the present invention, the mold may consist of more than one part, wherein the interior volume is defined by a lower part.
[0231] The term “sol gel process” as used herein refers to a method for producing solid materials from small molecules. In the present case, the method is used for the fabrication of porous materials such as aerogels, xerogels and/or kryogels. The process involves conversion of monomers as precursors into a colloidal solution, the so-called sol, that subsequently reacts to an integrated network, the so-called gel, of either discrete particles or network polymers. In this chemical procedure, the sol gradually evolves towards the formation of a gel-like diphasic system containing both a liquid phase and solid phase whose morphologies range from discrete particles to continuous polymer networks. This gel-like diphasic system is called gel. Particularly, the gel encapsulates or surrounds the solvent within pores which are connected to one another, i.e. the pores form an interpenetrating network. Removal of the remaining liquid phase, i.e. the solvent, requires a drying process, which is typically accompanied by a certain amount of shrinkage and densification. The rate at which the solvent can be removed is ultimately determined by the distribution of porosity in the gel. The ultimate microstructure of the final component will clearly be strongly influenced by changes imposed upon the structural template during this phase of processing.
[0232] The term “body” as used herein refers to a solid object formed by an identifiable collection of matter, which may be constrained by an identifiable boundary, and may move or may be moved as a unit by translation or rotation, in 3-dimensional space.
[0233] The term “porous” as used herein refers to material characteristics of having pores. As the solvent may be removed from the gel either with the gel being or remaining within the mold or after the gel is removed from the mold, the term “porous” covers both pores being filled with a liquid, particularly, the solvent, or a gas such as air. The pores may be connected to one another so as to form a type of network.
[0234] The term “coating” as used herein refers to a covering that is applied to the inner surfaces of the lower part of the mold. Particularly, the coating may be applied at least to those areas of the lower part intended to come into contact with the precursors of the porous material and the body made thereof. Needless to say, the coating may be applied to the total inner surfaces of the lower part defining the interior volume.
[0235] The term “electrically dissipative” as used herein refers to material characteristics, wherein electric charges are allowed to flow to ground but more slowly in a more controlled manner if compared to electrically conductive materials.
[0236] The term “non-sticky” as uses herein refers to characteristics wherein one part does not adhere to another part. Thus, both parts are in loose contact to one another. According to the present invention, the coating does not stick to the gel formed or resulting from the precursors filled into the mold. In case the solvent used with the sol gel process is removed with the gel being within the mold, the coating is configured not to stick to the thus formed body in order to allow the body being removed from the mold.
[0237] The terms “width” and “length” of the shape of the body as used herein refer to dimensions perpendicular to a height or thickness of the shape of the body.
[0238] The term “opening area” as used herein refers to the area of an opening defined by the boundary of the opening.
[0239]
[0240] Step 12 is repeated so as to form a plurality of gel bodies 12. Particularly, step S12 may be repeated any number of times as appropriate and depending on the respective application. The gel bodies 12 may be formed as slabs, wherein the slabs comprise a length of at least 10 cm and a width of at least 10 cm. For practical reasons, the upper limit for the length and/or the width may be 200 cm or even 100 cm. The slabs comprise a thickness of at least 0.5 mm. For practical reasons, the upper limit for the thickness may be 25.0 mm, 20.0 mm or 15.0 mm. Subsequently, in step S14, the gel bodies 12 are removed from the mold 10. With other words, the gel bodies 12 from each mold 10 or in case a single mold 10 is used, the gel bodies 12 are removed from the mold 10 in a subsequent order after a predetermined time in which the gel body/bodies 12 is/are formed from the precursors of the porous material. Further, the solvent S may be recycled or re-extracted by means of a re-extraction device.
[0241] In step S16, the gel bodies 12 are arranged adjacent to one another. In step S18, a spacer 14 is provided between two adjacent gel bodies 12 so as to provide a clearance therebetween. It has to be noted that steps S16 and S18 may be carried out at the same time. In step S20, the solvent S is removed from the gel bodies 12. The removing of the solvent S from the gel bodies 12 is performed by means of supercritical drying or convective drying. The removing may take place in an autoclave or oven. In the example shown in
[0242]
[0243] The grid assembly 16 may be modified as follows. The first openings 22 and/or the second openings 24 may be arranged in an irregular pattern. The first openings 22 and/or the second openings 24 may comprise different opening areas. The first openings 22 and/or the second openings 24 may comprise different shapes. The first openings 22 and/or the second openings 24 may comprise a circular, oval, elliptical, polygonal or polygonal including rounded edges, shape.
[0244]
[0245]
[0246]
[0247]
[0248] In step S16, the gel bodies 12 are arranged adjacent to one another such that the surface 32 including the protrusions 30 of one of the gel bodies 12 faces a surface 34 without protrusions of the respective adjacent body 12. Thus, by arranging the gel bodies 12 adjacent to one another, the spacer 14 formed by the protrusions 30 is automatically provided between two adjacent gel bodies 12 so as to provide a clearance therebetween. With other words, steps S16 and step S18 are combined. In step S20, the solvent S is removed from the gel bodies 12 as described above, i.e. by means of convective or supercritical drying. In the example shown in
[0249] The bodies 12 may be modified as follows by modifying the mold 10 shown in
[0250]
[0251]
[0252]
[0253]
[0254]
[0255]
CITED LITERATURE
[0256] WO 00/24799 [0257] WO 2009/027310 [0258] WO 2016/150684 A1 [0259] US 2005/0159497 A1