CN114477949A - Preparation method of gel felt, equipment for preparing gel felt and aerogel felt - Google Patents

Preparation method of gel felt, equipment for preparing gel felt and aerogel felt Download PDF

Info

Publication number
CN114477949A
CN114477949A CN202210110127.3A CN202210110127A CN114477949A CN 114477949 A CN114477949 A CN 114477949A CN 202210110127 A CN202210110127 A CN 202210110127A CN 114477949 A CN114477949 A CN 114477949A
Authority
CN
China
Prior art keywords
felt
gel
fiber
impregnation tank
sol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202210110127.3A
Other languages
Chinese (zh)
Other versions
CN114477949B (en
Inventor
张继承
刘喜宗
李静
杨红霞
陈帅
曹二伟
王琰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gongyi Van Research Yihui Composite Material Co Ltd
Original Assignee
Gongyi Van Research Yihui Composite Material Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Gongyi Van Research Yihui Composite Material Co Ltd filed Critical Gongyi Van Research Yihui Composite Material Co Ltd
Priority to CN202210110127.3A priority Critical patent/CN114477949B/en
Publication of CN114477949A publication Critical patent/CN114477949A/en
Application granted granted Critical
Publication of CN114477949B publication Critical patent/CN114477949B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00—Compositions for artificial stone, not containing binders
    • C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
    • C04B14/06—Quartz; Sand
    • C04B14/064—Silica aerogel
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
    • D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06H—MARKING, INSPECTING, SEAMING OR SEVERING TEXTILE MATERIALS
    • D06H7/00—Apparatus or processes for cutting, or otherwise severing, specially adapted for the cutting, or otherwise severing, of textile materials
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Civil Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a preparation method of a gel felt and equipment for preparing the gel felt, wherein silica sol and a gel catalyst are respectively injected into an impregnation tank; unreeling the fiber roll felt, and combining the continuous fiber felt with the silica sol and the gel catalyst through an impregnation tank; vertically conveying the fiber felt combined with the catalytic sol downwards under the action of gravity to remove redundant glue solution, and transferring the fiber felt to a moving element for gelation to form a silicon dioxide gel felt; and rolling the silicon dioxide gel felt into a rolled silicon dioxide gel felt or cutting the rolled silicon dioxide gel felt into a sheet silicon dioxide gel felt, and then drying to obtain the aerogel felt. The present invention controls the amount of impregnation by gravity transfer to produce a silica aerogel blanket having a uniform pore structure and uniform and excellent thermal insulation properties.

Description

Preparation method of gel felt, equipment for preparing gel felt and aerogel felt
Technical Field
The invention relates to the field of aerogel preparation, in particular to a method and equipment for continuously preparing a silica gel felt filled with a solvent, wherein the silica gel felt is used for preparing a silica aerogel felt related product.
Background
Aerogel refers to a solid structure that does not collapse after the liquid in the gel structure is replaced with gas. The silica aerogel is a continuous three-dimensional network structure formed by mutually polymerizing nano-scale particles, and the thermal conductivity efficiency, the convection heat transfer efficiency and the radiation heat transfer efficiency of the silica aerogel are effectively limited due to the special nano-scale micropores and a skeleton structure, so that the silica aerogel has a very low thermal conductivity coefficient, and is a solid material with the lowest thermal conductivity coefficient in the world at present.
Generally, aerogels are obtained by preparing a hydrogel from a silica precursor such as water glass or Tetraethylorthosilicate (TEOS) and removing the liquid component from the hydrogel without destroying the microstructure. Silica aerogels include three conventional forms of powder, granule and monolith. The aerogel felt or aerogel sheet is prepared by compounding the silica aerogel and the fibers, and is applied to the fields of industrial heat preservation and the like.
The prior art employs continuously combining a sol with a gel inducing agent to form a catalyzed sol, and combining a fibrous material with the catalyzed sol at a predetermined rate on a moving element for gelation to form a gel sheet. However, in actual production, when the sol and the gel catalyst are combined with the fiber material on the moving member, the sol and the gel catalyst are not sufficiently impregnated into the fiber material, and there is a case where the impregnation is not uniform, resulting in deterioration of the thermal insulation performance of the aerogel product. Therefore, in the prior art, the amount of the sol and the gel catalyst is increased to achieve sufficient impregnation, but the sol and the gel catalyst exceeding the impregnation amount overflow on the moving element, the overflowing sol catalyzed by the gel catalyst forms a gel solid block (or powder) on the moving element, which causes process failure of a mechanical operation processing device, the gel solid block on the conveyor belt is also partially adhered to a subsequently produced gel felt, the gel felt is rolled or cut into gel pieces to be stacked after the gel felt is continuously produced to carry out batch aging, drying and other processes, and the adhered gel solid block causes wrinkles, pits and breakage of upper and lower layers of felt in a gel block area, so that the quality of a subsequently produced aerogel felt product is affected.
Disclosure of Invention
The invention aims to provide a preparation method of a gel felt, which is used for preparing a silica gel roll felt filled with a solvent in a continuous mode and reducing the influence on the gel felt caused by the retention and agglomeration of a sol on a conveyor belt in the gelation process of a catalyzed sol combined with a fiber felt on a moving element.
A method of making a gel mat, the method comprising:
1) respectively injecting the silica sol and the gel catalyst into an impregnation tank;
2) unreeling a fiber rolling felt, and before silica sol gel, enabling a continuous fiber felt to pass through an impregnation tank to combine silica sol and a gel catalyst to form a fiber felt combined with catalytic sol;
3) before the silica sol is gelled, the fiber felt combined with the catalytic sol is vertically conveyed downwards under the action of gravity; and transferring the fiber mat combined with the catalytic sol to a moving element for movement and gelation to form a gel mat.
Further, in step 1):
silica sol and gel catalyst are respectively injected into the impregnation tank, the catalytic sol formed by mixing in the impregnation tank is respectively injected into the impregnation tank, the injection rate can be controlled by controlling respective control devices to further prevent the viscosity before impregnation from being increased, and the control of the gel time and the physical properties of silica aerogel are facilitated.
The silica sol and the gel catalyst are injected into the impregnation tank and may mix to form a catalytic sol, and a portion of the silica sol and the gel catalyst may also be present without mixing. In order to slow down the viscosity increase of the catalytic sol formed by mixing the silica sol and the gel catalyst in the impregnation tank, the silica sol and the gel catalyst are respectively injected into the impregnation tank from the top end and the bottom end of the impregnation tank or from two side ends of the impregnation tank.
The precursor of the silicon dioxide sol is silicon-containing alkoxide compounds, and comprises one or two of tetramethyl orthosilicate, tetraethyl orthosilicate, methyl triethyl orthosilicate, dimethyl diethyl orthosilicate, tetrapropyl orthosilicate, tetraisopropyl orthosilicate, tetrabutyl orthosilicate, tetra-sec-butyl orthosilicate, tetra-tert-butyl orthosilicate, tetrahexyl orthosilicate and forty-dialkyl orthosilicate. Preferably, the silica precursor of the present invention is selected from tetramethyl orthosilicate, tetraethyl orthosilicate, or a mixture thereof.
The silica sol is prepared by mixing a silica precursor with an alcohol, the alcohol being one of methanol, ethanol, isopropanol, and butanol. In addition, the hydrolysis and polycondensation steps of silicon can be catalyzed by alkali or acid with strong negative charges, and hydrolysis and polycondensation are simultaneously generated in the hydrolysis-condensation reaction process of the silicon source, only the difference of high or low degree of maturity exists. Generally, the hydrolysis rate is higher than the polycondensation rate under acidic conditions, the hydrolysis reaction is accelerated under acidic conditions, the polycondensation rate is higher than the hydrolysis rate under alkaline conditions, and the polycondensation reaction is accelerated under alkaline conditions. And catalyzing the reaction process of hydrolyzing the silica precursor to form the silica sol by using an acidic catalyst, wherein the acidic catalyst comprises one or more selected from nitric acid, hydrochloric acid and hydrofluoric acid. The gel catalyst adopts an alkaline catalyst which can be one of sodium hydroxide or potassium hydroxide and ammonium hydroxide, the content of the alkaline catalyst enables the pH of the sol to be 7-11, and when the pH of the silica sol exceeds the range, the gel rate is too slow.
Further, the fibers in the fiber mat are one or a combination of two or more of the following group of fiber materials: quartz fibers, glass fibers, high silica fibers, carbon fibers, pre-oxidized fiber, mullite fibers, basalt fibers, silicon carbide fibers, silicon nitride fibers, alumina fibers, boron nitride fibers.
Further, in step 2):
the combination in the step 2) comprises combining the silica sol and the gel catalyst by passing the continuous fiber mat through an impregnation tank in a soaking or spraying manner.
Specifically, the step 2) of combining the silica sol and the gel catalyst with the continuous fiber mat passing through the impregnation tank means that the silica sol and the gel catalyst are combined by immersing the continuous moving fiber mat into the impregnation tank.
The continuously moving fiber mat is combined with the silica sol and gel catalyst by soaking into an impregnation tank and with the catalytic sol formed by mixing in the impregnation tank. The impregnation can be more sufficient by the immersion impregnation. The continuous moving fiber mat combined with the silica sol and gel catalyst by soaking into the impregnation tank may have a problem that the silica sol combined with the fiber mat and the gel catalyst are not sufficiently mixed, and the silica sol and the gel catalyst may be supplemented by providing a squeeze roller in the impregnation tank.
The silica sol and the gel catalyst are respectively injected into the impregnation tank, and part of the silica sol and the gel catalyst are mixed to form the catalytic sol before the silica sol and the gel catalyst are combined with the fiber mat in a soaking way, so that the fiber mat and the catalytic sol are combined before the catalytic sol gel is formed by mixing, and the influence of the gelation viscosity increase of the silica sol on the combination with the fiber mat is avoided.
Or specifically, the step 2) of combining the silica sol and the gel catalyst with the continuous fiber mat through the impregnation tank is to spray the silica sol and the gel catalyst onto the continuously moving fiber mat in the impregnation tank respectively to combine the fiber mat with the silica sol and the gel catalyst respectively, and the silica sol and the gel catalyst are mixed on the fiber mat to form the catalytic sol. The injection rate can be controlled by controlling respective control devices through respectively spraying the mixture on the fiber felt, so that the viscosity before spraying is prevented from being improved, and the gel time and the physical properties of the silicon dioxide aerogel can be controlled; however, the separate spraying may have a problem that the silica sol and the gel catalyst combined with the fiber mat are not sufficiently mixed, and the mixing of the silica sol and the gel catalyst may be supplemented by providing a squeeze roll in the impregnation tank.
Further, the speed of the fiber felt in the impregnation tank in the step 2) combined with the catalytic sol through the impregnation tank is required to meet the condition that the combination time of the fiber felt and the catalytic sol is 0.1-10 min.
Further, in step 3):
and 3) when the fibrofelt combined with the catalytic sol in the step 3) is vertically conveyed downwards to the tail end of the continuous fibrofelt under the action of gravity and leaves away from the felt body supply device, the tail end of the fibrofelt is descended downwards through a lifting mechanism, the descending speed is consistent with the unreeling speed of the fibrofelt unreeled through the felt body supply device before gum dipping, so that the fibrofelt integrally keeps vertical descending at a constant speed, and the condition that the tail end of the fibrofelt vertically falls under the action of gravity only under the action of no tension force is avoided.
The end of the fiber felt refers to a fiber felt body continuously supplied to the impregnation tank by unwinding and unwinding a roll of 15-100 meters of fiber felt, and when the fiber felt body is separated from the felt body supply device at the end of unwinding, the fiber felt body is separated from the felt body supply device to a fiber felt section positioned between the fiber felts of the lifting mechanism.
In the step 3), because the viscosity of the catalytic sol formed by the silica sol and the gel catalyst is increased, the fiber mat needs to be vertically conveyed downwards under the action of gravity before the catalytic sol gel is formed.
Further, in the step 3), in order to prevent excessive impregnation and ensure proper impregnation level, the fiber mat combined with the catalytic sol is vertically conveyed downwards under the action of gravity, the height and the conveying speed meet the requirement that the fiber mat moves for 0.1-10min under the action of gravity, too short time can result in no separation of the surplus impregnation amount and surplus impregnation amount on the fiber mat, and too long time can result in excessive separation of the surplus impregnation amount and shortage of the impregnation amount on the fiber mat.
4) Further, the method also comprises a step 4) of rolling the gel felt obtained in the step 3) into a rolled silicon dioxide gel felt or cutting the rolled silicon dioxide gel felt into a sheet silicon dioxide gel felt.
Further, in step 2), step 3) and step 4):
further, the relationship among the unreeling speed of unreeling the fiber mat in the step 2), the speed of passing the continuous fiber mat through the impregnation tank in combination with the catalytic sol before the silica sol gel, the transfer speed of vertically and downwardly transferring the fiber mat combined with the catalytic sol in the step 3) under the action of gravity, the moving speed on the moving element, and the reeling speed of reeling the silica gel mat in the step 4) into the rolled silica gel mat is as follows: the winding speed is consistent with the unwinding speed, the conveying speed, the moving speed and the speed of passing through the impregnation tank, so that continuous fiber felt tensioning is ensured, and the fiber felt breakage caused by overlarge tensioning force in the conveying process is avoided.
According to another aspect of the present invention, there is provided an apparatus for preparing a gel mat, the apparatus comprising:
the impregnation tank is positioned at a high position and is used for combining the catalytic sol and the fiber felt;
the felt body supply device is connected to one side of the impregnation tank and used for unreeling the fiber roll felt to supply continuous felt bodies to the impregnation tank;
a silica sol injection device for injecting the silica sol into the impregnation tank so as to be mixed with the gel catalyst in the impregnation tank to be combined with the fiber mat body;
a gel catalyst injection device for injecting a gel catalyst into the impregnation tank so as to bond the silica sol and the fiber mat body with the gel catalyst;
and the moving element is positioned at a low position and forms a height difference with the impregnation tank at a high position, and is used for moving the fiber felt which is vertically conveyed downwards through the impregnation tank at the high position under the action of gravity and gelatinizing the fiber felt to form the gel felt.
Further, the silica sol injection device and the gel catalyst injection device are respectively provided with a flow control device for controlling the flow of the silica sol and the flow of the gel catalyst.
Further, the fiber mat is a roll mat wound in the form of a roll, and the roll mat is unreeled at a constant rate by a mat body supplying apparatus to be supplied to the impregnation tank.
The two side ends of the impregnation tank are respectively provided with a carrier roller for facilitating the movement of the fiber felt into and out of the impregnation tank.
The fiber felt is combined with the silica sol and the gel catalyst through the impregnation tank, and in order to ensure that the fiber felt is fully and uniformly impregnated, the extrusion roller is arranged in the impregnation tank to promote the catalytic sol, the silica sol and the gel catalyst to be uniformly impregnated into the fiber felt, so that saturated impregnation is ensured.
Further, the squeezing roller in the impregnation tank is provided with a driving device for driving the fiber felt to be conveyed in the impregnation tank by the rotation of the squeezing roller.
Further, the impregnation tank is provided with a feed inlet, the silica sol and the gel catalyst are respectively connected with the feed inlet and are continuously injected into the impregnation tank, the silica sol is connected with the first feed inlet, the gel catalyst is connected with the second feed inlet, the first feed inlet and the second feed inlet can be respectively arranged at the top end and the bottom end of the impregnation tank, can also be respectively arranged at two side ends, and can also be simultaneously arranged at the top end or the bottom end or the same side end; the injection amount keeps the liquid level of the catalytic sol formed by mixing the silicon dioxide sol and the gel catalyst in the impregnation tank to slightly overflow on the fiber felt, so as to ensure that the fiber felt can be fully soaked. In order to avoid the viscosity increase of the catalytic sol formed by mixing the silica sol and the gel catalyst in the impregnation tank, the first feed port and the second feed port are preferably arranged at the top end and the bottom end of the impregnation tank or at the two side ends of the impregnation tank respectively.
Or the dipping tank is internally provided with spraying equipment, the silica sol and the gel catalyst are respectively sprayed on the fiber felt, and the liquid level of the catalytic sol mixed by the silica sol and the gel catalyst in the dipping tank is kept on the fiber felt to slightly overflow, so that the fiber felt can be fully dipped.
Further, the apparatus for preparing a gel mat further comprises:
the gel felt winding equipment is used for winding the gel felt into a rolled silicon dioxide gel felt;
or further comprising a gel mat cutting apparatus for cutting the gel mat into a sheet-like silica gel mat.
Further, the device also comprises a lifting mechanism arranged at the other side of the impregnation tank, and the lifting mechanism can be used for descending the tail end of the fiber felt downwards at a preset speed.
Furthermore, the lifting mechanism also comprises a clamping mechanism used for clamping the tail end of the fiber felt, and the clamping mechanism clamps and fixes the tail end of the fiber felt so that the fiber felt can be conveyed at a constant speed along with the lifting mechanism at a preset speed.
Further, the lifting mechanism is a chain transmission type lifting platform, the tail end of the fiber felt combined with the catalytic sol after unreeling is placed on the lifting mechanism, a worker moves the tail end of the fiber felt downwards at a preset speed by using the lifting mechanism, the lifting mechanism drives the gel felt to stop when the gel felt reaches the height of the moving element, and the moving element moves and gels the tail end of the fiber felt.
Further, a recovery tank is arranged below the fiber felt which is vertically conveyed downwards under the action of gravity, and the recovery tank recovers the silica sol which is separated from the fiber felt under the action of gravity and exceeds the gum dipping amount. The recovered silica sol has a low viscosity and can be re-injected into the impregnation tank.
The aerogel felt is prepared by the equipment or the method, and has a uniform pore structure, uniform and excellent heat insulation performance, uniform and good surface appearance and no crushing, pits or wrinkles.
Has the advantages that: the method for preparing a silica gel mat according to the present invention can vertically move a fiber mat passing through an impregnation tank in combination with a silica sol and a gel catalyst downward by gravity transfer, in this process, since the silica sol has a low viscosity, the silica sol exceeding the impregnation amount is separated from the fiber mat by gravity, and then prevent the silica sol and gel catalyst that overflows that the excessive impregnation causes from taking place the gelation on the moving element and agglomerating on the moving element and influencing the machinery and gel product quality, then gelate and make the gel felt on the moving element again, the invention can make the sol remove the surplus sol and gel on the moving element under the action of gravity through controlling the gel time, make the silica aerogel felt with homogeneous pore structure and homogeneous and excellent heat-insulating property, homogeneous good surface appearance.
Drawings
FIG. 1 is a schematic view of embodiment 1 of the present invention;
FIG. 2 is a schematic view of embodiment 2 of the present invention;
FIG. 3 is a schematic view of embodiment 3 of the present invention;
FIG. 4 is a schematic view of embodiment 4 of the present invention;
FIG. 5 is a schematic view of embodiment 5 of the present invention;
in the figure: 1. silica sol injection equipment; 2. a gel catalyst injection device; 3. a flow control device; 4. a moving element; 5. a felt supply device; 6. a fiber mat; 7. a carrier roller; 8. an impregnation tank; 9. a squeeze roll; 10. winding equipment; 11. a lifting mechanism; 12. a cutting device; 13. gel sheets; 14. an injection device; 15. a recovery tank.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
It is to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1:
an apparatus for preparing a gel mat, as shown in fig. 1, comprises
An impregnation tank 8 located at a high level for combining the silica sol, the gel catalyst and the fiber mat 6;
a felt body supply device 5 connected to one side of the impregnation tank 8 for unreeling the fiber roll felt to supply a continuous felt body to the impregnation tank 8;
a silica sol injection apparatus 1 for injecting a silica sol into the impregnation tank 8 so as to mix the silica sol with a gel catalyst to be combined with the fiber mat 6;
a gel catalyst injection device 2 for injecting a gel catalyst into the impregnation tank 8 so as to mix the gel catalyst with the silica sol to be combined with the fiber mat 6;
the silica sol injection device 1 and the gel catalyst injection device 2 are respectively provided with a flow control device 3 for controlling the flow of the silica sol and the flow of the gel catalyst;
a moving member 4 located at a lower position and forming a height difference with the impregnation tank 8 located at a higher position, the height difference being used for vertically conveying the fiber mat passing through the impregnation tank located at the higher position downwards under the action of gravity, and the fiber mat combined with the catalytic sol is moved by the moving member 4 and is gelled on the moving member 4;
and the gel felt rolling equipment 10 is used for rolling the silica gel felt into a rolled silica gel felt.
The dipping tank 8 is provided with a feed inlet, silica sol and gel catalyst are respectively connected into the dipping tank 8 with the continuity of the feed inlet, the silica sol is connected with a first feed inlet and the gel catalyst is connected with a second feed inlet, and the first feed inlet and the second feed inlet are respectively arranged at the top end and the bottom end of the dipping tank 8.
And carrier rollers 7 are respectively arranged at two side ends of the impregnation tank 8 so as to facilitate the movement of the fiber felt into and out of the impregnation tank.
The fiber felt 6 is combined with the silica sol and the gel catalyst through the impregnation tank 8, and in order to ensure that the fiber felt is fully and uniformly impregnated, the extrusion roller 9 is arranged in the impregnation tank to promote the catalytic sol, the silica sol and the gel catalyst to be uniformly impregnated into the fiber felt 6, so that saturated impregnation is ensured.
The apparatus for making the gel mat further comprises: a lifting mechanism 11 arranged on the other side of the impregnation tank 8 opposite the supply device, said lifting mechanism 11 being capable of being used to drop the fibre mat end downwards at a predetermined speed. The lifting mechanism 11 comprises a clamping mechanism (not shown in the figure) for clamping the tail end of the fibrofelt, the clamping mechanism clamps and fixes the tail end of the fibrofelt to enable the fibrofelt to be conveyed at a constant speed along with the lifting mechanism 11, the lifting mechanism 11 is a chain transmission type lifting platform, the tail end of the fibrofelt combined with the catalytic sol after being unreeled is placed on the lifting mechanism 11, the clamping mechanism of the lifting mechanism 11 clamps and fixes the tail end of the fibrofelt, a worker moves the lifting platform downwards to move the tail end of the fibrofelt downwards at a preset speed, the lifting mechanism 11 drives the gel felt to the height of the moving element 4 to stop, and the moving element 4 moves and gelatinizes the tail end of the fibrofelt.
A method of making a gel mat, the method comprising:
1) tetraethoxysilane is used as a silicon dioxide precursor, tetraethoxysilane, ethanol and water are uniformly mixed, wherein the molar ratio of the tetraethoxysilane: ethanol: water = 1: 3: 6; adding sulfuric acid, adjusting the pH value to be 4, and uniformly stirring to obtain silicon dioxide sol; the gel catalyst is alkaline catalyst ammonia water; respectively injecting the silica sol and the gel catalyst into an impregnation tank 8 through a flow control device 3, wherein the flow ratio of the silica sol to the gel catalyst meets the requirement that the pH of the sol after being fully mixed in the impregnation tank 8 is 8, and the silica sol and the gel catalyst are respectively injected into the impregnation tank 8 from the top end and the bottom end of the impregnation tank 8;
2) unreeling a glass fiber roll felt, supplying a continuously unreeled fiber felt 6 to a dipping tank 8 by a felt body supply device 5, before silica sol is gelled, soaking the continuous fiber felt 6 into catalytic sol formed by mixing silica sol and a gel catalyst in the dipping tank 8 and silica sol and a gel catalyst through the dipping tank 8, compounding the glass fiber felt 6 with the catalyzed sol, the silica sol and the gel catalyst, and extruding the fiber felt 6 by an extrusion roller 9 in the dipping tank 8 to promote the catalyzed sol to be fully compounded with the fiber felt 6 and fully mix the sol with the gel catalyst;
3) the fiber mat 6 combined with the catalytic sol is vertically conveyed downwards under the action of gravity before the silica sol is gelled, and the fiber mat combined with the catalytic sol is transferred onto the moving element 4, and the fiber mat moves and is gelled on the moving element 4;
4) rolling the silica gel felt into a roll-shaped silica gel felt;
wherein, the unreeling speed of unreeling the fiber coiled felt in the step 2), the speed of combining the continuous fiber felt 6 with the catalytic sol through the impregnation tank 8 before the silica sol gel, the conveying speed of vertically conveying the fiber felt combined with the catalytic sol downwards under the action of gravity in the step 3), the moving speed on the moving element, and the reeling speed of reeling the silica gel felt into the coiled silica gel felt in the step 4) have the relation of: the rolling speed is consistent with the unreeling speed, the conveying speed, the moving speed and the speed of the fiber felt passing through the dipping tank 8, the speed meets the condition that the fiber felt 6 is soaked in the catalytic sol and the catalyzed sol in the dipping tank 8 for 1min, the time of the fiber felt 6 in the gravity action conveying process is 1min, so that the residual silicon dioxide sol on the fiber felt 6 is removed, and then the fiber felt is gelatinized in the moving process of the moving element 4.
And 3) when the fibrofelt combined with the catalytic sol in the step 3) is vertically conveyed downwards to the tail end of the continuous fibrofelt under the action of gravity and leaves the felt body supply device 5, the tail end of the fibrofelt is descended downwards through the lifting mechanism 11, the descending speed is consistent with the unreeling speed of a fibrofelt before gum dipping, and the condition that the tail end of the fibrofelt vertically falls under the action of gravity only under the action of no tension force is avoided.
Aging, hydrophobic modification, solvent replacement and supercritical drying are carried out on the silica gel felt prepared by the method to prepare the aerogel felt with hydrophobicity, wherein the aging step comprises the steps of aging the rolled gel felt at 70 ℃ for 1h, carrying out surface modification by hexamethyldisilazane, carrying out solvent replacement on the modified gel felt for 3 times, then placing the silica gel felt in supercritical drying equipment for supercritical drying, and replacing alcohol and water in the pore structure of the silica gel felt by CO2After discharge of CO2Obtaining the silica aerogel felt.
Example 2:
the present embodiment is different from embodiment 1 in that: as shown in figure 2 of the drawings, in which,
an apparatus for producing a gel mat, a gel mat cutting apparatus 12 for cutting a silica gel mat into a sheet-like silica gel mat, is not provided with a lifting mechanism 11.
A preparation method of the gel felt comprises the following steps: 4) and cutting the silica gel felt into a sheet-shaped silica gel felt.
The aerogel felt is prepared by aging, hydrophobic modification, solvent replacement and supercritical drying of the gel felt obtained by the method. The aerogel blanket is in the form of a sheet.
Example 3:
the present embodiment is different from embodiment 1 in that: as shown in figure 3 of the drawings,
the utility model provides an equipment for preparing gel felt, the flooding jar 8 is provided with the feed inlet, and silica sol and gel catalyst are connected the injection flooding jar 8 of feed inlet continuation respectively in, and first feed inlet is connected to silica sol, gel catalyst connection second feed inlet, and first feed inlet and second feed inlet set up respectively in the relative both sides end of flooding jar 8.
A recovery tank 15 is arranged below the fibrofelt which is vertically conveyed downwards under the action of gravity, the recovery tank 15 recovers silica sol which is separated from the fibrofelt 6 under the action of gravity and exceeds the gum dipping amount, and the recovery tank 15 is communicated with the dipping tank 8.
A preparation method of the gel felt comprises the following steps: 1) the silica sol and the gel catalyst are injected into the impregnation tank 8 from both side ends of the impregnation tank, respectively.
The catalyst sol recovered by the recovery tank 15 is injected into the impregnation tank 8 from the bottom end of the impregnation tank 8.
The aerogel felt is prepared by aging, hydrophobic modification, solvent replacement and supercritical drying of the gel felt obtained by the method.
Example 4:
the present embodiment is different from embodiment 1 in that: as shown in figure 4 of the drawings,
an apparatus for preparing a gel mat,
the dipping tank 8 is internally provided with a spraying device 14 which sprays the silica sol and the gel catalyst onto the fiber felt 6 from the top end of the dipping tank 8 respectively, and keeps the liquid level of the catalytic sol mixed by the silica sol and the gel catalyst in the dipping tank 8 slightly overflowed on the fiber felt 6 so as to ensure that the fiber felt 6 can be fully dipped.
A preparation method of a gel felt comprises the following steps of 2) unreeling a glass fiber roll felt, supplying a continuously unreeled fiber felt 6 to a dipping tank 8 by a felt body supply device 5, enabling the continuous fiber felt 6 to pass through the dipping tank 8, respectively spraying silica sol and a gel catalyst on the fiber felt 6 in the dipping tank 8 through a spraying device 14, extruding the fiber felt 6 by an extruding roller 9 in the dipping tank 8, compounding the glass fiber felt 6 with a catalyzed sol, and promoting the catalyzed sol to be fully compounded with the fiber felt 6 by the extruding roller 9.
The aerogel felt is prepared by aging, hydrophobic modification, solvent replacement and supercritical drying of the gel felt obtained by the method.
Example 5:
this embodiment is different from embodiment 4 in that: as shown in figure 5 of the drawings,
an apparatus for preparing a gel mat, a gel mat cutting apparatus 12, for cutting a silica gel mat into a sheet-like silica gel mat.
A preparation method of the gel felt comprises the following steps: 4) and cutting the silica gel felt into a sheet-shaped silica gel felt.
The aerogel felt is prepared by aging, hydrophobic modification, solvent replacement and supercritical drying of the gel felt obtained by the method. The aerogel blanket is in the form of a sheet.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention, the scope of the present invention is defined by the appended claims, and all structural changes that can be made by using the contents of the description and the drawings of the present invention are intended to be embraced therein.

Claims (10)

1. A preparation method of a gel felt is characterized by comprising the following steps: the method comprises the following steps:
respectively injecting the silica sol and the gel catalyst into an impregnation tank;
unreeling a fiber rolling felt, and before silica sol gel, enabling a continuous fiber felt to pass through an impregnation tank to combine silica sol and a gel catalyst to form a fiber felt combined with catalytic sol;
before the silica sol is gelled, the fiber felt combined with the catalytic sol is vertically conveyed downwards under the action of gravity; and transferring the fiber mat with the bound catalytic sol to a moving element for movement and gelation.
2. The method of making a gel mat according to claim 1, wherein: and in the step 1), the silica sol and the gel catalyst are respectively injected into the impregnation tank from the top end and the bottom end of the impregnation tank or from two side ends of the impregnation tank.
3. The method of making a gel mat according to claim 1, wherein: the combination in the step 2) comprises combining the silica sol and the gel catalyst by passing the continuous fiber mat through an impregnation tank in a soaking or spraying manner.
4. The method of making a gel mat according to claim 1, wherein: in the step 2), the speed of the fiber felt combined with the silica sol and the gel catalyst in the impregnation tank passing through the impregnation tank is required to meet the condition that the combination time of the fiber felt and the catalyst sol is 0.1-10 min; the fiber felt combined with the catalytic sol in the step 3) is vertically conveyed downwards under the action of gravity, and the height and the conveying speed meet the requirement that the fiber felt moves for 0.1-10min under the action of gravity.
5. The method of making a gel mat according to claim 1, wherein: and 3) when the fiber felt combined with the catalytic sol in the step 3) is vertically conveyed downwards to the tail end of the fiber felt under the action of gravity and leaves the felt body supply device, the tail end of the fiber felt is descended downwards at a preset speed through a lifting mechanism, and the preset speed is consistent with the unreeling speed of the fiber coiled felt through the felt body supply device, so that the whole fiber felt is vertically conveyed downwards at a constant speed.
6. The method of making a gel mat according to claim 1, wherein: and (4) rolling the gel felt obtained in the step 3) into a roll-shaped gel felt or cutting the gel felt into a sheet-shaped gel felt.
7. An apparatus for making a gel mat, characterized by: the apparatus comprises:
the impregnation tank is positioned at a high position and is used for combining the catalytic sol and the fiber felt;
the felt body supply device is connected to one side of the impregnation tank and used for unreeling the fiber roll felt to supply continuous fiber felt to the impregnation tank;
a silica sol injection device for injecting the silica sol into the impregnation tank so as to be mixed with the gel catalyst in the impregnation tank to be combined with the fiber mat;
a gel catalyst injection device for injecting a gel catalyst into the impregnation tank so as to combine the silica sol with the fiber mat;
and the moving element is positioned at a low position and forms a height difference with the impregnation tank at a high position, and is used for moving the fiber felt which is vertically conveyed downwards through the impregnation tank at the high position under the action of gravity and gelatinizing the fiber felt to form the gel felt.
8. The apparatus for making a silica gel blanket of claim 7 wherein: the apparatus further includes a lift mechanism disposed on the other side of the impregnation tank from the supply apparatus, the lift mechanism being operable to drop the fiber mat ends downwardly at a predetermined velocity.
9. The apparatus for making a silica gel blanket of claim 7 wherein: the equipment also comprises gel felt rolling equipment which is used for rolling the gel felt into a roll-shaped gel felt;
or a gel mat cutting apparatus for cutting the gel mat into sheet-like gel mats.
10. Aerogel blanket made by the apparatus or method of any of claims 1-9, wherein: and carrying out subsequent or aging or hydrophobic modification or solvent replacement and drying processes on the obtained gel felt to obtain the aerogel felt.
CN202210110127.3A 2022-01-29 2022-01-29 Preparation method of gel felt, equipment for preparing gel felt and aerogel felt Active CN114477949B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210110127.3A CN114477949B (en) 2022-01-29 2022-01-29 Preparation method of gel felt, equipment for preparing gel felt and aerogel felt

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210110127.3A CN114477949B (en) 2022-01-29 2022-01-29 Preparation method of gel felt, equipment for preparing gel felt and aerogel felt

Publications (2)

Publication Number Publication Date
CN114477949A true CN114477949A (en) 2022-05-13
CN114477949B CN114477949B (en) 2023-02-14

Family

ID=81478106

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210110127.3A Active CN114477949B (en) 2022-01-29 2022-01-29 Preparation method of gel felt, equipment for preparing gel felt and aerogel felt

Country Status (1)

Country Link
CN (1) CN114477949B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114702295A (en) * 2022-05-20 2022-07-05 巩义市泛锐熠辉复合材料有限公司 Aerogel composite material and preparation method thereof
CN114773027A (en) * 2022-06-16 2022-07-22 巩义市泛锐熠辉复合材料有限公司 Aerogel felt prepared at low cost and preparation method thereof
CN115094623A (en) * 2022-07-25 2022-09-23 巩义市泛锐熠辉复合材料有限公司 Module occupying type gel tank and gel method
CN116393052A (en) * 2023-03-31 2023-07-07 广东埃力生科技股份有限公司 Aerogel product, and preparation method and preparation system thereof
CN117552201A (en) * 2023-11-10 2024-02-13 广东埃力生科技股份有限公司 Aerogel felt preparation system and preparation method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107531495A (en) * 2016-01-19 2018-01-02 株式会社Lg化学 The manufacture method and manufacture device of airsetting film
CN107531496A (en) * 2016-01-19 2018-01-02 株式会社Lg化学 The manufacture method and manufacture device of airsetting film
CN107531497A (en) * 2016-01-19 2018-01-02 株式会社Lg化学 The manufacture method and manufacture device of airsetting film
CN107848813A (en) * 2016-02-19 2018-03-27 株式会社Lg化学 For manufacturing the apparatus and method of airsetting film
CN110770168A (en) * 2017-08-24 2020-02-07 株式会社Lg化学 Method of manufacturing silica aerogel blanket and apparatus for manufacturing the same
CN113195432A (en) * 2019-09-18 2021-07-30 株式会社Lg化学 Aerogel blanket and method of making same
CN113896505A (en) * 2021-09-30 2022-01-07 巩义市泛锐熠辉复合材料有限公司 Method for discontinuously producing aerogel felt

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107531495A (en) * 2016-01-19 2018-01-02 株式会社Lg化学 The manufacture method and manufacture device of airsetting film
CN107531496A (en) * 2016-01-19 2018-01-02 株式会社Lg化学 The manufacture method and manufacture device of airsetting film
CN107531497A (en) * 2016-01-19 2018-01-02 株式会社Lg化学 The manufacture method and manufacture device of airsetting film
CN107848813A (en) * 2016-02-19 2018-03-27 株式会社Lg化学 For manufacturing the apparatus and method of airsetting film
US20180179075A1 (en) * 2016-02-19 2018-06-28 Lg Chem, Ltd. Apparatus and method for manufacturing aerogel sheet
CN110770168A (en) * 2017-08-24 2020-02-07 株式会社Lg化学 Method of manufacturing silica aerogel blanket and apparatus for manufacturing the same
CN113195432A (en) * 2019-09-18 2021-07-30 株式会社Lg化学 Aerogel blanket and method of making same
CN113896505A (en) * 2021-09-30 2022-01-07 巩义市泛锐熠辉复合材料有限公司 Method for discontinuously producing aerogel felt

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114702295A (en) * 2022-05-20 2022-07-05 巩义市泛锐熠辉复合材料有限公司 Aerogel composite material and preparation method thereof
CN114702295B (en) * 2022-05-20 2023-02-28 巩义市泛锐熠辉复合材料有限公司 Aerogel composite material and preparation method thereof
CN114773027A (en) * 2022-06-16 2022-07-22 巩义市泛锐熠辉复合材料有限公司 Aerogel felt prepared at low cost and preparation method thereof
CN114773027B (en) * 2022-06-16 2023-06-27 巩义市泛锐熠辉复合材料有限公司 Aerogel felt prepared at low cost and preparation method thereof
CN115094623A (en) * 2022-07-25 2022-09-23 巩义市泛锐熠辉复合材料有限公司 Module occupying type gel tank and gel method
CN115094623B (en) * 2022-07-25 2023-06-30 巩义市泛锐熠辉复合材料有限公司 Module occupying type gel groove and gel method
CN116393052A (en) * 2023-03-31 2023-07-07 广东埃力生科技股份有限公司 Aerogel product, and preparation method and preparation system thereof
CN116393052B (en) * 2023-03-31 2023-12-26 广东埃力生科技股份有限公司 Aerogel product, and preparation method and preparation system thereof
CN117552201A (en) * 2023-11-10 2024-02-13 广东埃力生科技股份有限公司 Aerogel felt preparation system and preparation method

Also Published As

Publication number Publication date
CN114477949B (en) 2023-02-14

Similar Documents

Publication Publication Date Title
CN114477949B (en) Preparation method of gel felt, equipment for preparing gel felt and aerogel felt
CN114541059A (en) Equipment for preparing gel felt, preparation method of gel felt and aerogel
KR101748532B1 (en) Preparation method and apparatus of aerogel sheet
JP6909875B2 (en) Manufacturing method of silica airgel blanket and its manufacturing equipment
CN113896505B (en) Method for discontinuously producing aerogel felt
JP7071542B2 (en) How to make an airgel blanket
US20070152363A1 (en) Gel production via multi-stream mixing
CN107848813B (en) Apparatus and method for manufacturing aerogel sheet
EP3296265B1 (en) Method and apparatus for preparing aerogel sheet
KR102583201B1 (en) Preparation method for aerogel blanket
EP3878812B1 (en) Aerogel blanket and manufacturing method therefor
JP2018538221A (en) Airgel sheet manufacturing method and apparatus
CN106567248A (en) Preparation method for preparing super-hydrophobic cross-linked silica fiber foams
CN114773027B (en) Aerogel felt prepared at low cost and preparation method thereof
KR101928538B1 (en) Aerogel composite
CN115043408B (en) Flexible silica aerogel, aerogel felt and preparation method thereof
CN114653529B (en) Device and method for preparing silica aerogel felt and silica aerogel felt
CN116446106A (en) Equipment for preparing gel felt, preparation method of gel felt and aerogel felt
CN114986943B (en) Aerogel waste felt recycling equipment and method
CN113737515B (en) Aerogel structure and method for producing same
CN114956099B (en) Gel material surface defect treatment device and treatment method
CN115124319B (en) High-compression silicon dioxide aerogel, aerogel felt and preparation method thereof
CN115073127B (en) Apparatus and method for simultaneous production of gel felt and modified gel
CN112795180A (en) Preparation method of enhanced automobile motor controller top cover
JP3792841B2 (en) Method and apparatus for producing catalyst carrier

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant