CN115819973B - Rapid composite preparation method for large-size continuous aerogel coiled material - Google Patents
Rapid composite preparation method for large-size continuous aerogel coiled material Download PDFInfo
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- CN115819973B CN115819973B CN202211376759.0A CN202211376759A CN115819973B CN 115819973 B CN115819973 B CN 115819973B CN 202211376759 A CN202211376759 A CN 202211376759A CN 115819973 B CN115819973 B CN 115819973B
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 239000004964 aerogel Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 27
- 238000013329 compounding Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000032683 aging Effects 0.000 claims abstract description 18
- 238000012986 modification Methods 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims abstract description 17
- 238000000352 supercritical drying Methods 0.000 claims abstract description 14
- 238000005470 impregnation Methods 0.000 claims abstract description 12
- 238000007598 dipping method Methods 0.000 claims abstract description 11
- 239000004744 fabric Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 238000004804 winding Methods 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- -1 polyethylene Polymers 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- XUIMIQQOPSSXEZ-IGMARMGPSA-N silicon-28 atom Chemical compound [28Si] XUIMIQQOPSSXEZ-IGMARMGPSA-N 0.000 claims description 4
- 229920006231 aramid fiber Polymers 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-RNFDNDRNSA-N silicon-32 atom Chemical compound [32Si] XUIMIQQOPSSXEZ-RNFDNDRNSA-N 0.000 claims description 3
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000012774 insulation material Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- Y—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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Silicon Compounds (AREA)
Abstract
The invention discloses a rapid composite preparation method of a large-size continuous aerogel coiled material, and belongs to the technical field of heat insulation materials. Preparing high-reactivity low-temperature impregnating solution at low temperature, preparing a fiber coiled material rewinding body from a large-size continuous fiber coiled material and a net-shaped diversion cloth roll, carrying out impregnation by using the impregnating solution to realize rapid compounding, then carrying out rapid reaction aging, supercritical drying and modification treatment to obtain a large-size continuous aerogel coiled material rewinding body, and independently separating to obtain a large-size continuous aerogel coiled material. The method realizes the aging of the quick reaction gel by cooling and heating the sol after dipping, eliminates the volatilization and combustibility of organic components in the production environment, and realizes the purpose of environment-friendly quick compounding.
Description
Technical Field
The invention relates to a rapid composite preparation method of a large-size continuous aerogel coiled material, and belongs to the technical field of heat insulation materials.
Background
The industrial energy-saving technology is rapidly developed, and aerogel is used as an optimal heat insulation material and an optimal solution for energy saving effect, so that a great amount of industrial demands of aerogel materials are promoted. In solving the aerogel product production that industry field used, aerogel presents multiple product forms such as sheet, bulk, coiled material and abnormal shape component, and wherein coiled material application occasion is wider, and its good flexibility crimping performance gives the laminating ability that well adapts to multiple different structure appearance, and the cuttability is good, and it is more nimble to use. The existing aerogel coiled material is mainly prepared by crawler-type on-line dipping and compounding, the technological method has the advantages of high dipping and compounding speed, and the crawler-type on-line dipping and compounding process is used for compounding sol containing a large amount of organic solvents with a fiber matrix; the open length of the crawler belt is up to tens of meters, and although the organic solvent centralized collecting cover is additionally arranged, a large amount of organic solvents volatilize when the crawler belt is immersed and laid in an open mode, the volatilization is continuous and durable, combustible gas is enriched, and the problems of high production safety, occupational sanitation safety and the like are caused. In view of this, there is a need to solve the problem of eliminating volatilization of organic components in the impregnation and compounding process while ensuring the rapid impregnation and compounding efficiency, and thus a rapid compounding preparation method for large-sized continuous aerogel coiled materials has been proposed.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a preparation method of a large-size continuous aerogel coiled material, which has the advantages of rapid forming, less solvent use, low cost and the like, is an optimal heat insulation material for industrial heat insulation, and has industrial energy-saving heat insulation application value.
A rapid composite preparation method of a large-size continuous aerogel coiled material comprises the following steps:
(1) Preparing an impregnating solution: according to the mol ratio of 1 (3-10), 1.5-3, 0.005-0.01 and 0.005-0.02, weighing tetraethoxysilane, ethanol, water, ammonium fluoride and ammonia water, fully cooling the materials to the low temperature of 0-10 ℃, uniformly mixing the tetraethoxysilane, the ethanol and the water, and adding ammonium fluoride and ammonia water catalyst to prepare high-reactivity low-temperature impregnating solution;
(2) Rewinding: winding the large-size continuous fiber coiled material and the netlike diversion cloth onto a central roller tool of a rewinding device together to form a fiber coiled material rewinding body;
(3) And (3) quick compounding: vertically placing the fiber coiled material rewinding body and the central roller tool into an impregnating device, vacuumizing, and then sucking impregnating liquid into the impregnating device for impregnation to realize rapid compounding;
(4) Fast reaction aging: taking out the composite rewinding body from the impregnating device, coating and packaging by using a protective bag, and finishing reaction aging in an aging temperature environment;
(5) Supercritical drying: carrying out supercritical drying treatment on the aged composite rewinding body, and doping a modifying reagent into a drying kettle through a drying medium after drying is finished to carry out modification treatment, so as to obtain a large-size continuous aerogel coiled material rewinding body;
(6) And (3) separating rolls: the aerogel coiled material rewinding body comprises a reticular diversion cloth and an aerogel coiled material which is supported after the steps are processed, the reticular diversion cloth and the aerogel coiled material are respectively wound, the reticular diversion cloth is independently wound, the aerogel coiled material is independently wound, and the aerogel coiled material is the obtained large-size continuous aerogel coiled material.
Preferably, the tetraethoxysilane is one of silicon-28 tetraethoxysilane, silicon-32 tetraethoxysilane and silicon-40 tetraethoxysilane.
Preferably, the fiber type of the fiber coiled material is one of glass fiber, high silica fiber, aramid fiber, graphite fiber, aluminum silicate fiber, aluminum oxide fiber, mullite fiber, non-woven fabric and the like.
Preferably, the large-size continuous fiber coiled material has a width of 0.5-2 m and a continuous length of 1-200 m.
Preferably, the center roller tool is a tool with a fixed circular chassis at one side of a center roller shaft; the center roller is of a hollow structure, and the inner diameter of the center roller is matched with the air expansion shaft of the rewinding device.
Preferably, the impregnating device is a closed sealing device.
Preferably, the vacuum degree of the vacuumizing is-0.08 to-0.095 MPa; the time of vacuumizing the impregnating solution before impregnation is 30-60 min; the reaction time after the dipping is 0.5 to 2 hours.
Preferably, the protective bag is a polyethylene plastic cylindrical bag resistant to 100 ℃; the aging temperature is 30-60 ℃ and the aging time is 12-48 h.
Preferably, the supercritical drying is carbon dioxide supercritical drying.
Preferably, the modifying agent is one of trimethylmethoxysilane, trimethylchlorosilane, methyltrimethoxysilane and dimethyldimethoxysilane.
Preferably, the conditions of the modification treatment include: the modification duration temperature is 50-60 ℃, and the modification duration treatment time is 0.5-4 h.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts a vacuum rapid compounding method in a closed tool, and after the sol cooling in the step (1) and the dipping in the subsequent step, the sol is heated in the step (4), so that the aging of the rapid reaction gel is realized, the volatilization and combustibility of organic components in the production environment are eliminated, and the purpose of environment-friendly rapid compounding is realized. The high-reactivity impregnating solution is mainly influenced by concentration and proportion of tetraethoxysilane, water, a catalyst and the like to form a rapid crosslinking reaction system, sol can be rapidly converted into gel, and the gel solution is unstable, easy to gel and difficult to store in the preparation process.
(2) The invention realizes low-cost rapid molding, wherein the impregnation compounding is rapid, avoids the phenomena of volatilization of organic solvent, overflow of glue solution in the crawler belt and the like in the conventional crawler belt type impregnation compounding method, improves the utilization rate of raw materials, and cancels solvent replacement and the like.
(3) The method has the characteristics of rapid molding, simple operation, production space saving, low cost and the like, and is a safe, environment-friendly, rapid and low-cost aerogel molding method.
Drawings
FIG. 1 is a flow chart of a rapid composite preparation of a large-size continuous aerogel coil of the present invention.
Detailed Description
In order to make the above features and advantages of the present invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
(1) Preparing an impregnating solution: evenly mixing silicon-28 type tetraethoxysilane, ethanol and water, adding ammonium fluoride and ammonia water catalyst according to the proportion, wherein the proportion is calculated according to the molar ratio, and fully cooling the mixture to 0 ℃ before the mixture is prepared to prepare the high-reactivity low-temperature impregnating solution, wherein the molar ratio of silicon-28 type tetraethoxysilane to ethanol to water is calculated by the molar ratio of ammonium fluoride to ammonia water=1:3:3:0.005:0.01.
(2) Rewinding: winding a large-size continuous glass fiber coiled material and a net-shaped diversion cloth onto a central roller tool together to form a fiber coiled material rewinding body with a certain diameter; the breadth is 0.5m, and the continuous length is 50m.
(4) And (3) quick compounding: and (3) vertically placing the rewinding body in the step (2) and the central roller tool into an impregnating device with a certain diameter, vacuumizing the impregnating device with the vacuum degree of-0.08 MPa, vacuumizing for 30min, sucking impregnating liquid into the impregnating device, and reacting for 0.5h to finish the rapid impregnation and compounding.
(4) Fast reaction aging: and (3) taking out the composite rewinding body by the dipping device, coating and packaging by using a polyethylene plastic cylindrical bag resistant to 100 ℃, and finishing reaction aging for 24 hours at 30 ℃.
(5) Supercritical drying: and (3) carrying out carbon dioxide supercritical drying treatment on the composite rewinding body, and doping a trimethylmethoxysilane modifying reagent into a drying kettle through a drying medium after the drying is finished, wherein the modification duration temperature is 50 ℃, and the modification duration treatment time is 0.5h, so as to obtain the large-size continuous aerogel coiled material rewinding body.
(6) And (3) separating rolls: and (3) placing the aerogel coiled material rewinding body into a rewinding device, respectively winding, independently winding the guide net, and independently winding the aerogel coiled material to prepare the final large-size continuous aerogel coiled material.
Product performance test: preparation of the gas-off gel coil Density 206kg/m 3 The breadth is 0.5m, the continuous length is 50m, and the room temperature thermal conductivity is 0.019W/(K.m).
Example 2
(1) Preparing an impregnating solution: evenly mixing silicon-32 type tetraethoxysilane, ethanol and water, adding ammonium fluoride and ammonia water catalyst according to the proportion, wherein the proportion is calculated according to the molar ratio, and fully cooling to 5 ℃ before the preparation and mixing, so as to prepare the high-reactivity low-temperature impregnating solution.
(2) Rewinding: winding a large-size continuous high silica fiber coiled material and a net-shaped diversion cloth onto a central roller tool together to form a fiber coiled material rewinding body with a certain diameter; the breadth is 1m, and the continuous length is 100m.
(5) And (3) quick compounding: and (3) vertically placing the rewinding body in the step (2) and the central roller tool into an impregnating device with a certain diameter, vacuumizing the impregnating device with the vacuum degree of-0.09 MPa, vacuumizing for 45min, and then sucking impregnating liquid into the impregnating device, and reacting for 1h to finish impregnation rapid compounding.
(4) Fast reaction aging: and (3) taking out the composite rewinding body by the dipping device, coating and packaging by using a polyethylene plastic cylindrical bag resistant to 100 ℃, and finishing reaction aging for 48 hours at 40 ℃.
(5) Supercritical drying: and (3) carrying out carbon dioxide supercritical drying treatment on the composite rewinding body, and doping a trimethylchlorosilane modifying reagent into a drying kettle through a drying medium after the drying is finished, wherein the modification duration temperature is 55 ℃, and the modification duration treatment time is 4 hours, so as to obtain the large-size continuous aerogel coiled material rewinding body.
(6) And (3) separating rolls: and (3) placing the aerogel coiled material rewinding body into a rewinding device, respectively winding, independently winding the guide net, and independently winding the aerogel coiled material to prepare the final large-size continuous aerogel coiled material.
Product performance test: preparation of the gas-off gel coil Density 201kg/m 3 The breadth is 1m, the continuous length is 100m, and the room temperature thermal conductivity is 0.021W/(K.m).
Example 3
(1) Preparing an impregnating solution: evenly mixing silicon-40 type tetraethoxysilane, ethanol and water, adding ammonium fluoride and ammonia water catalyst according to the proportion, wherein the proportion is calculated according to the molar ratio, and the silicon-40 type tetraethoxysilane, ethanol, water and ammonium fluoride are mixed according to the molar ratio of ammonia water=1:10:1.5:0.01:0.02, and fully cooling to 10 ℃ before the mixing, so as to prepare the high-reactivity low-temperature impregnating solution.
(2) Rewinding: winding a large-size continuous aramid fiber coiled material and a net-shaped diversion cloth onto a central roller tool together to form a fiber coiled material rewinding body with a certain diameter; the breadth is 2m, and the continuous length is 200m.
(6) And (3) quick compounding: and (3) vertically placing the rewinding body in the step (2) and the central roller tool into an impregnating device with a certain diameter, vacuumizing the impregnating device with the vacuum degree of-0.095 MPa, vacuumizing for 60min, sucking impregnating liquid into the impregnating device, and reacting for 2h to finish the impregnation rapid compounding.
(4) Fast reaction aging: and (3) taking out the composite rewinding body by the dipping device, coating and packaging by using a polyethylene plastic cylindrical bag resistant to 100 ℃, and finishing reaction aging for 12 hours at 60 ℃.
(5) Supercritical drying: and (3) carrying out carbon dioxide supercritical drying treatment on the composite rewinding body, and doping a methyltrimethoxysilane modifying reagent into a drying kettle through a drying medium after the drying is finished, wherein the modification duration temperature is 60 ℃, and the modification duration treatment time is 2 hours, so that the large-size continuous aerogel coiled material rewinding body is obtained.
(6) And (3) separating rolls: and (3) placing the aerogel coiled material rewinding body into a rewinding device, respectively winding, independently winding the guide net, and independently winding the aerogel coiled material to prepare the final large-size continuous aerogel coiled material.
Product performance test: preparation of the gas-off gel coil Density 213kg/m 3 The breadth is 2m, the continuous length is 200m, and the room temperature thermal conductivity is 0.0025W/(K.m).
Comparative example
This comparative example is substantially the same as example 1 except that the impregnating solution prepared in step (1) was prepared at normal temperature, and the normal temperature impregnating solution was used in the subsequent impregnating process.
Product performance test: preparation of the gas gel coil Density 198kg/m 3 The breadth is 0.5m, the continuous length is 50m, and the room temperature thermal conductivity is 0.039W/(K.m).
As is clear from the comparison of examples and comparative examples, the comparative examples are high reactive impregnating solutions prepared at normal temperature, and the high reactive impregnating solutions have partial gel reaction in the subsequent use process, so that the density of the product is lower and the heat insulation effect is poorer.
The invention is not described in detail in a manner known to those skilled in the art.
Although the present invention has been described with reference to the above embodiments, it should be understood that the invention is not limited thereto, and that modifications and equivalents may be made thereto by those skilled in the art, which modifications and equivalents are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (10)
1. The rapid composite preparation method of the large-size continuous aerogel coiled material is characterized by comprising the following steps of:
according to the mol ratio of 1 (3-10), 1.5-3, 0.005-0.01 and 0.005-0.02, weighing tetraethoxysilane, ethanol, water, ammonium fluoride and ammonia water, fully cooling the materials to the low temperature of 0-10 ℃, uniformly mixing the tetraethoxysilane, the ethanol and the water, and adding ammonium fluoride and ammonia water catalyst to prepare high-reactivity low-temperature impregnating solution;
winding the large-size continuous fiber coiled material and the netlike diversion cloth onto a central roller tool of a rewinding device together to form a fiber coiled material rewinding body;
vertically placing the fiber coiled material rewinding body and the central roller tool into an impregnating device, vacuumizing, and then sucking the impregnating liquid into the impregnating device for impregnation to realize rapid compounding;
taking out the composite rewinding body from the impregnating device, coating and packaging by using a protective bag, and finishing reaction aging in an aging temperature environment;
carrying out supercritical drying treatment on the aged composite rewinding body, and doping a modifying reagent into a drying kettle through a drying medium after drying is finished to carry out modification treatment, so as to obtain a large-size continuous aerogel coiled material rewinding body;
the method is characterized in that the aerogel coiled material rewinding body is placed into a rewinding device and comprises net-shaped guide cloth and aerogel coiled materials which are supported after being processed in the steps, the net-shaped guide cloth is wound respectively, the aerogel coiled materials are wound independently, and the aerogel coiled materials are wound independently, so that the obtained large-size continuous aerogel coiled materials are obtained.
2. The method of claim 1, wherein the ethyl orthosilicate is one of type silicon-28 ethyl orthosilicate, type silicon-32 ethyl orthosilicate, and type silicon-40 ethyl orthosilicate.
3. The method of claim 1, wherein the fibrous web is one of a glass fiber, a high silica fiber, an aramid fiber, a graphite fiber, an aluminum silicate fiber, an aluminum oxide fiber, a mullite fiber, a nonwoven fabric, and the like.
4. The method of claim 1, wherein the large-size continuous fiber web has a size of 0.5 to 2m in width and a continuous length of 1 to 200m.
5. The method of claim 1, wherein the center roll tooling is tooling with a fixed circular chassis on one side of a center roll shaft; the central roller is of a hollow structure, and the inner diameter of the central roller is matched with the air expansion shaft of the rewinding device; the dipping device is a closed sealing device.
6. The method of claim 1, wherein the evacuated vacuum level is-0.08 to-0.095 MPa; the time of vacuumizing the impregnating solution before impregnation is 30-60 min; the reaction time after the dipping is 0.5 to 2 hours.
7. The method of claim 1, wherein the protective bag is a polyethylene plastic cylindrical bag resistant to 100 ℃; the aging temperature is 30-60 ℃ and the aging time is 12-48 h.
8. The method of claim 1, wherein the supercritical drying is carbon dioxide supercritical drying.
9. The method of claim 1, wherein the modifying agent is one of trimethylmethoxysilane, trimethylchlorosilane, methyltrimethoxysilane, dimethyldimethoxysilane.
10. The method of claim 1, wherein the conditions of the modification treatment comprise: the modification duration temperature is 50-60 ℃, and the modification duration treatment time is 0.5-4 h.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4342712A (en) * | 1979-06-28 | 1982-08-03 | Ube Industries, Ltd. | Process for producing continuous inorganic fibers |
| US5371138A (en) * | 1990-07-24 | 1994-12-06 | Tru Vue, Inc. | Ultraviolet blocking polysiloxane resin and process for making the same |
| JP2003215509A (en) * | 2002-01-24 | 2003-07-30 | Hoya Healthcare Corp | Method of manufacturing soft contact lens consisting of silicone hydrogel having hydrophilic surface and soft contact lens |
| JP2004035730A (en) * | 2002-07-03 | 2004-02-05 | Japan Polychem Corp | Resin composition and film obtained by molding it |
| CN1982522A (en) * | 2005-12-16 | 2007-06-20 | 航天材料及工艺研究所 | Fiberglass flow-guiding cloth and vacuum adsorption |
| CN107099117A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of fibre-reinforced aerogel-polymer composites and preparation method thereof |
| WO2019054544A1 (en) * | 2017-09-15 | 2019-03-21 | (주)티디엘 | Method for coating silicone on polyimide film |
| CN111102427A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Method for reinforcing and repairing metal pipeline by using carbon fiber cloth vacuum infusion technology |
| CN111778649A (en) * | 2020-06-18 | 2020-10-16 | 华陆工程科技有限责任公司 | Method for quickly preparing nano heat-insulating material through supercritical drying |
| CN112778707A (en) * | 2021-02-04 | 2021-05-11 | 宜宾三江机械有限责任公司 | Dielectric isolation material with thermosetting resin as matrix and preparation method thereof |
| CN114182157A (en) * | 2021-10-22 | 2022-03-15 | 南京钢铁股份有限公司 | Preparation method of hot-rolled steel strip for elastic check ring |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BR112013024886A2 (en) * | 2011-03-30 | 2017-08-01 | Toray Industries | prepreg, fiber reinforced composite material and method for making a fiber reinforced composite material |
| BR112017006480B1 (en) * | 2014-10-03 | 2022-10-11 | Aspen Aerogels, Inc. | REINFORCED AEROGEL COMPOUND AND METHOD TO PREPARE A REINFORCED AEROGEL COMPOUND |
-
2022
- 2022-11-04 CN CN202211376759.0A patent/CN115819973B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4342712A (en) * | 1979-06-28 | 1982-08-03 | Ube Industries, Ltd. | Process for producing continuous inorganic fibers |
| US5371138A (en) * | 1990-07-24 | 1994-12-06 | Tru Vue, Inc. | Ultraviolet blocking polysiloxane resin and process for making the same |
| JP2003215509A (en) * | 2002-01-24 | 2003-07-30 | Hoya Healthcare Corp | Method of manufacturing soft contact lens consisting of silicone hydrogel having hydrophilic surface and soft contact lens |
| JP2004035730A (en) * | 2002-07-03 | 2004-02-05 | Japan Polychem Corp | Resin composition and film obtained by molding it |
| CN1982522A (en) * | 2005-12-16 | 2007-06-20 | 航天材料及工艺研究所 | Fiberglass flow-guiding cloth and vacuum adsorption |
| CN107099117A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of fibre-reinforced aerogel-polymer composites and preparation method thereof |
| WO2019054544A1 (en) * | 2017-09-15 | 2019-03-21 | (주)티디엘 | Method for coating silicone on polyimide film |
| CN111102427A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Method for reinforcing and repairing metal pipeline by using carbon fiber cloth vacuum infusion technology |
| CN111778649A (en) * | 2020-06-18 | 2020-10-16 | 华陆工程科技有限责任公司 | Method for quickly preparing nano heat-insulating material through supercritical drying |
| CN112778707A (en) * | 2021-02-04 | 2021-05-11 | 宜宾三江机械有限责任公司 | Dielectric isolation material with thermosetting resin as matrix and preparation method thereof |
| CN114182157A (en) * | 2021-10-22 | 2022-03-15 | 南京钢铁股份有限公司 | Preparation method of hot-rolled steel strip for elastic check ring |
Non-Patent Citations (7)
| Title |
|---|
| Electrochemical and physical evaluations of coil coatings on metal-coated steels for roofing applications;J.N. Murray，等;《Progress in Organic Coatings》;第47卷(第2期);第136-146页 * |
| PDMS低温热解复合膜的制备与性能研究;郁蕉竹;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》(第08期);第B020-104页 * |
| Surface morphological and topographical analysis of multifunctional superhydrophobic sol-gel coatings;Satish A. Mahadik，等;《Ceramics International》;第47卷(第20期);第29475-29482页 * |
| 先驱体浸渍裂解工艺制备C_f/UHTC_p/SiC复合材料及其性能研究;王其坤;《中国博士学位论文全文数据库工程科技Ⅰ辑》(第04期);第B020-7页 * |
| 大张力缠绕成型用环氧树脂体系研究;刘丽;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》(第07期);第B016-225页 * |
| 木基柔性电子复合膜的制备及其在传感器中的应用;王怡仁，等;《复合材料学报》;第39卷(第8期);第4057-4064页 * |
| 石英纤维/有机硅树脂复合材料的制备及性能研究;杨燕;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》(第05期);第B020-108页 * |
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