CN115819973A - Rapid composite preparation method of large-size continuous aerogel coiled material - Google Patents

Rapid composite preparation method of large-size continuous aerogel coiled material Download PDF

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CN115819973A
CN115819973A CN202211376759.0A CN202211376759A CN115819973A CN 115819973 A CN115819973 A CN 115819973A CN 202211376759 A CN202211376759 A CN 202211376759A CN 115819973 A CN115819973 A CN 115819973A
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coiled material
fiber
aerogel
continuous
dipping
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CN115819973B (en
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周玉贵
盛锦华
张凡
陈玉玲
李鑫
李文静
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Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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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-reaction-activity low-temperature impregnation liquid at low temperature, rolling the large-size continuous fiber coiled material and the reticular flow guide cloth into a fiber coiled material rewind body, impregnating by using the impregnation liquid to realize rapid compounding, performing rapid reaction aging, supercritical drying and modification treatment to obtain the large-size continuous aerogel coiled material rewind body, and performing independent roll separation to obtain the large-size continuous aerogel coiled material. The method realizes rapid reaction gel aging through sol cooling and heating after dipping, eliminates volatile and combustible organic components in the production environment, and realizes the purpose of environment-friendly rapid composite molding.

Description

Rapid composite preparation method of large-size continuous aerogel coiled material
Technical Field
The invention relates to a rapid composite preparation method of a large-size continuous aerogel coiled material, belonging to the technical field of heat insulation materials.
Background
The industrial energy-saving technology is developed rapidly, and the aerogel is the best solution for the energy-saving effect as the best heat insulation material, so that the industrial mass demand of the aerogel material is promoted. In the aerogel goods production of solving industrial field to use, the aerogel presents multiple product forms such as sheet, bulk material, coiled material and heterotypic component, and wherein the coiled material application occasion is wider, and its good flexible curling performance gives the laminating ability that well is adapted to multiple different structure appearances, and cuttability is good, uses more in a flexible way. The prior aerogel coiled material is mainly prepared by crawler-type online dipping compounding, and the process method has the advantages of high dipping compounding speed, crawler-type online dipping compounding, compounding sol containing a large amount of organic solvents and a fiber matrix; the open length of the crawler belt is up to tens of meters, although the organic solvent centralized collection cover is additionally arranged, the open type dipping and laying on the crawler belt can cause volatilization of a large amount of organic solvent, the volatilization is continuous and lasting, and combustible gas is enriched, thereby bringing about the problems of great production safety, occupational health safety and the like. In view of this, it is necessary to solve the problem of eliminating the volatilization of organic components during the dipping composite production process and simultaneously ensure the rapid dipping composite efficiency, so a rapid composite preparation method for large-size continuous aerogel coiled materials is provided.
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 large-size continuous aerogel coiled material rapid composite preparation method comprises the following steps:
(1) Preparing an immersion liquid: weighing ethyl orthosilicate, ethanol, water, ammonium fluoride and ammonia water according to the molar ratio of 1 (3-10) to (1.5-3) to (0.005-0.01) to (0.005-0.02), fully cooling the substances to the low temperature of 0-10 ℃, uniformly mixing the ethyl orthosilicate, the ethanol and the water, and adding ammonium fluoride and an ammonia water catalyst to prepare high-reaction-activity low-temperature impregnation liquid;
(2) Rewinding: winding the large-size continuous fiber coiled material and the reticular flow guide cloth on a central roller tool of an rewinding device together, and winding the large-size continuous fiber coiled material and the reticular flow guide cloth into a fiber coiled material rewinding body;
(3) And (3) quick compounding: vertically placing the fiber coiled material reverse-wound body and the central roller tool into a dipping device, vacuumizing, and then sucking dipping liquid into the dipping device for dipping to realize rapid compounding;
(4) And (3) rapid reaction and aging: taking out the composite rewinding body from the dipping device, using a protection bag to carry out coating and packaging, and then finishing reaction aging in an aging temperature environment;
(5) Supercritical drying: carrying out supercritical drying treatment on the aged composite rewind body, and doping a modifying reagent into a drying kettle through a drying medium after drying to carry out modification treatment to obtain a large-size continuous aerogel coiled material rewind body;
(6) And (3) splitting: will the aerogel coiled material is rewound the body and is put into the device of rewinding, the aerogel coiled material is rewound the body and is included netted water conservancy diversion cloth and the aerogel coiled material that supports after above-mentioned step processing, and this two is the rolling respectively, and netted water conservancy diversion cloth independently becomes the lapping, and the independent lapping of aerogel coiled material, this aerogel coiled material is the continuous aerogel coiled material of jumbo size that obtains promptly.
Preferably, the ethyl orthosilicate is one of silicon-28 type ethyl orthosilicate, silicon-32 type ethyl orthosilicate and silicon-40 type ethyl orthosilicate.
Preferably, the fiber type of the fiber coiled material is one of glass fiber, high silica fiber, aramid fiber, graphite fiber, aluminum silicate fiber, alumina fiber, mullite fiber, non-woven fabric and the like.
Preferably, the size of the large-size continuous fiber coiled material is 0.5-2 m in width and 1-200 m in continuous length.
Preferably, the center roller tool is a tool with a fixed circular chassis at one side of a center roller shaft; the central roller is of a hollow structure, and the inner diameter of the central roller is matched with an air expansion shaft of the rewinding device.
Preferably, the steeping device is a closed sealing device.
Preferably, the vacuum degree of the vacuumizing is-0.08 to-0.095 MPa; the vacuumizing time of the impregnation liquid before impregnation is 30-60 min; the reaction time after dipping is 0.5 to 2 hours.
Preferably, the protection 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 trimethyl methoxy silane, trimethyl chlorosilane, methyl trimethoxy silane and dimethyl dimethoxy silane.
Preferably, the conditions of the modification treatment include: the continuous modification temperature is 50-60 ℃, and the continuous modification 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 in the step (1) is cooled and impregnated in the subsequent steps, the sol is heated in the step (4), so that the aging of rapid reaction gel is realized, the volatile and combustible organic components in the production environment are eliminated, and the purpose of environment-friendly rapid compound molding is realized. The high-reactivity impregnation liquid is mainly influenced by the concentration and proportion of ethyl orthosilicate, water, catalyst and the like to form a rapid crosslinking reaction system, can rapidly convert sol into gel, and the gel liquid is unstable, easy to gel and difficult to store in preparation.
(2) The invention realizes low-cost rapid molding, wherein the dipping compounding is rapid, the phenomena of organic solvent volatilization, glue solution overflow and the like in the crawler belt in the conventional crawler belt type dipping compounding method are avoided, the utilization rate of raw materials is improved, and solvent replacement and the like are cancelled.
(3) The method has the characteristics of quick forming, simple operation, production space saving, low cost and the like, and is a safe, environment-friendly, quick and low-cost aerogel forming method.
Drawings
FIG. 1 is a flow chart of the rapid compounding preparation of a large-size continuous aerogel coil according to the present invention.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
(1) Preparing an immersion liquid: uniformly mixing silicon-28 type tetraethoxysilane, ethanol and water, adding ammonium fluoride and an ammonia water catalyst according to a ratio, wherein the molar ratio of the silicon-28 type tetraethoxysilane, the ethanol, the water, the ammonium fluoride and the ammonia water is 0.005.
(2) Rewinding: winding the large-size continuous glass fiber coiled material and the reticular flow guide cloth together onto a center roller tool, and rolling into a fiber coiled material reverse-rolling body with a certain diameter; the width is 0.5m and the continuous length is 50m.
(4) And (3) quick compounding: vertically placing the rewinding body and the central roller tool in the step (2) into a dipping device with a certain diameter, vacuumizing the dipping device to a vacuum degree of-0.08 MPa for 30min, sucking the dipping liquid into the dipping device, and reacting for 0.5h to complete rapid dipping and compounding.
(4) And (3) rapid reaction and aging: and (4) taking out the composite body rewinding body by the dipping device in the step (3), coating and packaging by using a 100 ℃ resistant polyethylene plastic cylindrical bag, and finishing reaction and aging for 24 hours at the temperature of 30 ℃.
(5) Supercritical drying: and (3) carrying out carbon dioxide supercritical drying treatment on the composite roll-down body, and doping a trimethyl methoxysilane modified reagent into a drying kettle through a drying medium after drying is finished, wherein the modification continuous temperature is 50 ℃, and the modification continuous treatment time is 0.5h, so that the large-size continuous aerogel roll-down body is obtained.
(6) And (3) splitting: put into the back-rolling device with the aerogel coiled material back-rolling body, the rolling respectively, the independent lapping of water conservancy diversion net, the independent lapping of aerogel coiled material makes final jumbo size continuous aerogel coiled material.
And (3) product performance testing: the density of the prepared aerogel coiled material is 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 immersion liquid: uniformly mixing silicon-32 type tetraethoxysilane, ethanol and water, adding ammonium fluoride and an ammonia water catalyst according to a ratio, wherein the molar ratio of the silicon-32 type tetraethoxysilane, the ethanol, the water, the ammonium fluoride and the ammonia water is 0.005.
(2) Rewinding: winding the large-size continuous high silica fiber coiled material and the reticular flow guide cloth on a central roller tool together, and rolling into a fiber coiled material reverse-rolling body with a certain diameter; width 1m, continuous length 100m.
(5) And (3) quick compounding: vertically placing the middle rewinding body and the central roller tool in the step (2) into a dipping device with a certain diameter, vacuumizing the dipping device to a vacuum degree of-0.09 MPa for 45min, sucking the dipping liquid into the dipping device, and reacting for 1h to complete rapid dipping and compounding.
(4) And (3) rapid reaction and aging: and (3) taking out the composite rewinding body by using the dipping device, coating and packaging the composite rewinding body by using a 100 ℃ resistant polyethylene plastic cylindrical bag, and finishing reaction and aging for 48 hours at 40 ℃.
(5) Supercritical drying: and (3) carrying out carbon dioxide supercritical drying treatment on the composite roll-down body, and doping a trimethylchlorosilane modification reagent into a drying kettle through a drying medium after drying is finished, wherein the continuous modification temperature is 55 ℃, and the continuous modification treatment time is 4 hours, so that the large-size continuous aerogel roll-down body is obtained.
(6) And (3) splitting: put into the back-rolling device with the aerogel coiled material back-rolling body, the rolling respectively, the independent lapping of water conservancy diversion net, the independent lapping of aerogel coiled material makes final jumbo size continuous aerogel coiled material.
And (3) product performance testing: the density of the prepared aerogel coiled material is 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 immersion liquid: uniformly mixing silicon-40 type tetraethoxysilane, ethanol and water, adding ammonium fluoride and an ammonia water catalyst according to a ratio, wherein the molar ratio of the silicon-40 type tetraethoxysilane, the ethanol, the water, the ammonium fluoride and the ammonia water is = 1.5.
(2) Rewinding: winding a large-size continuous aramid fiber coiled material and a reticular flow guide cloth together onto a center roller tool, and rolling into a fiber coiled material reverse roll body with a certain diameter; the width is 2m, and the continuous length is 200m.
(6) And (3) quick compounding: and (3) vertically putting the middle rewinding body and the central roller tool in the step (2) into a dipping device with a certain diameter, vacuumizing the dipping device to a vacuum degree of-0.095 MPa for 60min, sucking the dipping liquid into the dipping device, and reacting for 2h to complete rapid dipping and compounding.
(4) And (3) rapid reaction and aging: and (4) taking out the composite body rewinding body by the dipping device in the step (3), coating and packaging by using a 100 ℃ resistant polyethylene plastic cylindrical bag, and finishing reaction and aging for 12 hours at 60 ℃.
(5) Supercritical drying: and (3) carrying out carbon dioxide supercritical drying treatment on the composite rolled body, and doping a methyltrimethoxysilane modified reagent into a drying kettle through a drying medium after drying is finished, wherein the continuous modification temperature is 60 ℃, and the continuous modification treatment time is 2 hours, so that the large-size continuous aerogel coiled material rolled body is obtained.
(6) And (3) splitting: put into the back-rolling device with the aerogel coiled material back-rolling body, the rolling respectively, the independent lapping of water conservancy diversion net, the independent lapping of aerogel coiled material makes final jumbo size continuous aerogel coiled material.
And (3) product performance testing: the density of the prepared aerogel coiled material is 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 impregnation solution prepared in step (1) was prepared at normal temperature, and the impregnation solution at normal temperature was used in the subsequent impregnation process.
And (3) product performance testing: the density of the prepared aerogel coiled material is 198kg/m 3 The breadth is 0.5m, the continuous length is 50m, and the room-temperature thermal conductivity is 0.039W/(K.m).
The comparative example of the comparative example shows that the comparative example is a high-reactivity impregnation liquid prepared at normal temperature, and in the subsequent use process, partial gel reaction occurs, so that the density of the product is lower and the heat insulation effect is poorer.
The invention has not been described in detail and is in part known to those of skill in the art.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. A large-size continuous aerogel coiled material rapid composite preparation method is characterized by comprising the following steps:
ethyl orthosilicate, ethanol, water, ammonium fluoride and ammonia water are weighed according to the molar ratio of 1 (3-10) to 1.5-3 to 0.005-0.01 to 0.005-0.02, the ethyl orthosilicate, the ethanol, the water, the ammonium fluoride and the ammonia water are fully cooled to the low temperature of 0-10 ℃, then the ethyl orthosilicate, the ethanol and the water are uniformly mixed, and ammonium fluoride and an ammonia water catalyst are added to prepare high-reaction-activity low-temperature impregnation liquid;
winding the large-size continuous fiber coiled material and the reticular flow guide cloth on a central roller tool of an rewinding device together, and winding the large-size continuous fiber coiled material and the reticular flow guide cloth into a fiber coiled material rewinding body;
vertically placing the fiber coiled material reverse-wound body and the central roller tool into a dipping device, vacuumizing, and then sucking the dipping liquid into the dipping device for dipping to realize rapid compounding;
taking out the composite rewinding body from the dipping device, using a protection bag to carry out coating and packaging, and then finishing reaction aging in an aging temperature environment;
carrying out supercritical drying treatment on the aged composite rewind body, and doping a modifying reagent into a drying kettle through a drying medium after drying to carry out modification treatment to obtain a large-size continuous aerogel coiled material rewind body;
will the aerogel coiled material is rewound the body and is put into the device of rewinding, the aerogel coiled material is rewound the body and is included netted water conservancy diversion cloth and the aerogel coiled material that supports after above-mentioned step processing, and the rolling respectively, the independent lapping of netted water conservancy diversion cloth, the independent lapping of aerogel coiled material, this aerogel coiled material is the continuous aerogel coiled material of jumbo size that obtains promptly.
2. The method of claim 1, wherein the ethyl orthosilicate is one of silicon-28 type ethyl orthosilicate, silicon-32 type ethyl orthosilicate, and silicon-40 type ethyl orthosilicate.
3. The method of claim 1, wherein the fiber type of the fiber coil is one of glass fiber, high silica fiber, aramid fiber, graphite fiber, alumina silicate fiber, alumina fiber, mullite fiber, non-woven fabric, and the like.
4. The method of claim 1, wherein the large continuous fiber web has dimensions of 0.5 to 2m width and 1 to 200m continuous length.
5. The method of claim 1, wherein the center roll tooling is a tooling with a fixed circular base plate on one side of the center roll axis; the central roller is of a hollow structure, and the inner diameter of the central roller is matched with an air expansion shaft of the rewinding device; the impregnation device is a closed sealing device.
6. The method of claim 1, wherein the degree of vacuum of the evacuation is from-0.08 to-0.095 MPa; the vacuumizing time of the impregnation liquid before impregnation is 30-60 min; the reaction time after dipping is 0.5 to 2 hours.
7. The method of claim 1 wherein said protective bag is a cylindrical bag of 100 ℃ resistant polyethylene plastic; 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 process comprise: the continuous modification temperature is 50-60 ℃, and the continuous modification treatment time is 0.5-4 h.
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