CN115974519B - Low-temperature-resistant flexible nano heat-insulating material and preparation method thereof - Google Patents
Low-temperature-resistant flexible nano heat-insulating material and preparation method thereof Download PDFInfo
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- 239000011810 insulating material Substances 0.000 title claims abstract description 56
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- 238000001035 drying Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 36
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 229910052782 aluminium Inorganic materials 0.000 claims description 8
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- 238000003756 stirring Methods 0.000 claims description 8
- 239000003365 glass fiber Substances 0.000 claims description 7
- QHQNYHZHLAAHRW-UHFFFAOYSA-N 2-trimethoxysilylethanamine Chemical group CO[Si](OC)(OC)CCN QHQNYHZHLAAHRW-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229920001778 nylon Polymers 0.000 claims description 6
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- 229920002748 Basalt fiber Polymers 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- MEWFSXFFGFDHGV-UHFFFAOYSA-N cyclohexyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C1CCCCC1 MEWFSXFFGFDHGV-UHFFFAOYSA-N 0.000 claims description 4
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 4
- ZFBOVYJITDWWBB-UHFFFAOYSA-N 3-triethoxysilylpropane-1,1,1-triamine Chemical compound CCO[Si](OCC)(OCC)CCC(N)(N)N ZFBOVYJITDWWBB-UHFFFAOYSA-N 0.000 claims description 3
- 229920002334 Spandex Polymers 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004759 spandex Substances 0.000 claims description 3
- OFYJUQNXYAHUOG-UHFFFAOYSA-N [ClH]1(C=CC=C1)=O Chemical compound [ClH]1(C=CC=C1)=O OFYJUQNXYAHUOG-UHFFFAOYSA-N 0.000 claims description 2
- 229920004934 Dacron® Polymers 0.000 claims 1
- 239000012774 insulation material Substances 0.000 abstract description 42
- 230000002209 hydrophobic effect Effects 0.000 abstract description 13
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- 230000001070 adhesive effect Effects 0.000 abstract description 11
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003063 flame retardant Substances 0.000 abstract description 8
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 4
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- 229920002215 polytrimethylene terephthalate Polymers 0.000 description 4
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- 229920004933 Terylene® Polymers 0.000 description 3
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical class C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 3
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Abstract
The invention discloses a low-temperature-resistant flexible nano heat-insulating material and a preparation method thereof, wherein the method comprises the following steps: mixing inorganic fibers and organic fibers in a certain proportion to form a hybrid fiber felt; mixing silicate, aminosilane, aldehyde, hexamethylenediamine and alcohol according to a certain weight ratio for reaction to obtain sol; mixing the sol with a gel catalyst to obtain a pre-gel solution; then placing the mixed fiber felt into a pre-gel solution to form a fiber wet felt of saturated adsorption gel; coating the surface of the wet fiber felt with a sealing film, aging in a constant temperature environment, removing the film, and drying; finally, a steam barrier film with back adhesive is attached to the surface of the nano heat insulation material, so that the low-temperature-resistant flexible nano heat insulation material is prepared. The heat insulation material prepared by the invention has good low temperature resistance and flexibility, and also has certain hydrophobic property and flame retardant property.
Description
Technical Field
The invention belongs to the technical field of heat insulation material manufacturing, and particularly relates to a low-temperature-resistant flexible nano heat insulation material and a preparation method thereof.
Background
The common heat insulating materials are generally classified into three types of organic, inorganic and metal materials, and the inorganic heat insulating materials have the characteristics of flame retardance and high strength when applied to a cold insulation project, but have the defects of insufficient low temperature resistance, high moisture absorption rate and high requirement on a moisture-proof layer; the organic material is applied to cold insulation engineering, has the advantages of low heat conductivity coefficient, light volume weight, low moisture absorption rate and easy installation, but also has the defects of low strength, poor ultralow temperature resistance (generally at more than or equal to-100 ℃), flammability, and degradation of toxic gas after combustion, and is unfavorable for environmental protection and safety; the metal material is not easy to form and process, is easy to transfer heat and has poor heat preservation performance. In conclusion, the existing cold insulation material has the defects of poor low temperature resistance, poor construction flexibility and the like in different degrees.
Disclosure of Invention
In view of the above, the present invention aims to solve at least one of the technical problems in the related art to some extent. Therefore, the embodiment of the invention provides a low-temperature-resistant flexible nano heat-insulating material and a preparation method thereof.
On the one hand, the embodiment of the invention provides a preparation method of a low-temperature-resistant flexible nano heat-insulating material, which comprises the following steps:
(1) Uniformly mixing inorganic fibers and organic fibers according to the weight ratio of (65-85) (15-35), and forming a hybrid fiber felt by a mechanical reinforcement method;
(2) Mixing silicate, aminosilane, aldehyde, hexamethylenediamine and alcohol uniformly, stirring at 25-55 ℃ for reaction, and ending the reaction when the pH value of the mixed solution reaches 6.5-7.5 to obtain sol; then mixing the sol and the gel catalyst at room temperature for 2-5 min to obtain a pre-gel solution;
(3) Placing the mixed fiber felt into a pre-gel solution, and soaking for 5-8 min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 5-10 h in a constant temperature environment of 40-60 ℃;
(5) Removing the film coated on the surface of the aged fiber wet felt, and drying to obtain a low-temperature-resistant flexible nano heat-insulating material prefabricated product;
(6) And adhering a steam barrier film with back glue to the surface of the low-temperature-resistant flexible nano heat-insulating material preform through roll forming to form the low-temperature-resistant flexible nano heat-insulating material.
According to the preparation method of the low-temperature-resistant flexible nano heat-insulating material, disclosed by the embodiment of the invention, the low-temperature resistance of a finished product material can be improved by adopting an organic-inorganic blend fiber base material with a certain proportion, and the crystallization embrittlement of a fiber framework structure at a low temperature is avoided; the flexibility in the molding process of the nano material can be improved by introducing the aminosilane, the aldehyde and the hexamethylenediamine in the sol process of the silicon-based aerogel, the crosslinking compactness in the forming process of the nano network structure is enhanced, the adhesive force of the sol and the fiber base material is enhanced, the overall flexibility of the material is increased, the low temperature resistance of the material is further enhanced, and the composite material with the flexibility and the cold transfer isolation is formed.
In some embodiments of the invention, in step (1), the hybrid fiber mat has a density of 120kg/m or less 3 Oxygen index > 32.
In some embodiments of the invention, in step (1), the weight ratio of the inorganic fibers to the organic fibers is preferably (75-85): (15-25).
In some embodiments of the present invention, in step (1), the inorganic fibers are glass fibers or basalt fibers having a diameter of 5 to 10 μm and a length of 3 to 10 cm; the organic fiber is any one of nylon, chlorlon, spandex, terylene, polyethylene terephthalate, polybutylene terephthalate or polypropylene terephthalate with the diameter of 5-14 mu m and the length of 5-10 cm.
In some embodiments of the invention, in step (2), the weight ratio of silicate, aminosilane, aldehyde, hexamethylenediamine, alcohol is: (50-80): (12-23): (5-18): (2-9): (100-160).
In some embodiments of the invention, in step (2), the silicate is any one of methyl silicate, ethyl silicate, methyltrimethoxysilane, propyltriethoxysilane, or cyclohexyltrimethoxysilane;
and/or the aminosilane is aminoethyltrimethoxy silane or triaminopropyl triethoxy silane;
and/or, the aldehyde is formaldehyde or trimesic aldehyde;
and/or the alcohol is methanol or ethanol.
In some embodiments of the invention, in step (2), the weight ratio of the sol to the gel catalyst is 100 (2-8);
further, the gel catalyst is 5-10wt% ammonia water or sodium hydroxide solution.
In some embodiments of the invention, in step (4), the constant temperature environment is provided by hot water and/or hot nitrogen.
In some embodiments of the invention, in step (5), the drying is any one of supercritical drying, atmospheric drying, or conduction drying;
further, the process conditions of the supercritical drying are as follows: CO 2 The flow rate of the catalyst is 120-260 kg/h, the drying temperature is 45-55 ℃, the drying pressure is 14.5-16.5 MPa, and the drying time is 5-8 h;
the normal pressure drying process conditions are as follows: the temperature of the hot nitrogen is 85-105 ℃ and the flow rate is 30m 3 And/h, the drying time is 10-18 h;
the process conditions of the conduction drying are as follows: n-hexane is used as a drying medium, the purity of the medium is 90-98%, the flow rate of the medium is 0.5-1.5 t/h, the temperature of the medium is 70-85 ℃, and the drying time is 8-15 h.
In some embodiments of the present invention, in the step (6), the vapor barrier film with back glue is formed by attaching a metal aluminum foil back glue with a thickness of 12-25 wires to any one of PI and modified ABS, PTFE, PPO, PE film with a thickness of 5-12 wires.
The embodiment of the invention also provides a low-temperature-resistant flexible nano heat-insulating material, which is prepared by the preparation method.
The features and advantages described above for the preparation method of the low temperature resistant flexible nano heat insulation material are also applicable to the low temperature resistant flexible nano heat insulation material, and are not described herein.
The invention has the advantages and beneficial effects that:
(1) In the embodiment of the invention, the composite material with flexibility and cold energy transmission isolation is prepared by adopting the organic-inorganic hybrid fiber base material and aerogel, wherein the organic-inorganic hybrid fiber can improve the low temperature resistance of the finished product material and avoid crystallization embrittlement of the fiber framework structure at low temperature; the amino silane, aldehyde and hexamethylenediamine are introduced in the sol process of the silicon-based aerogel, so that the flexibility in the molding process of the nano material can be improved, the crosslinking compactness in the forming process of the nano network structure is enhanced, the adhesive force of the sol and a fiber base material is enhanced, the overall flexibility of the material is increased, and the low temperature resistance of the material is further enhanced.
(2) In the preparation method of the low-temperature-resistant flexible nano heat-insulating material, the prepared heat-insulating material has the flame-retardant property by limiting the mixing ratio of the inorganic fibers and the organic fibers; in addition, the ageing process of the heat insulation material is carried out in a closed environment, so that volatilization of an organic solvent in the fiber wet felt can be avoided, and an ageing heat supply mode is optimized to improve operation safety.
Drawings
FIG. 1 is a process flow diagram of a low temperature resistant flexible nano heat insulation material according to an embodiment of the invention.
FIG. 2a is an optical photograph of the low temperature resistant flexible nano heat insulation material prepared in example 1 of the present invention.
Fig. 2b is an optical photograph of the low temperature resistant flexible nano heat insulation material prepared in example 1 of the present invention in the bending process after being immersed in liquid nitrogen for 48 hours.
Fig. 3 is a stress-strain curve diagram of the low temperature resistant flexible nano heat insulation material prepared in example 2 of the present invention before and after soaking in liquid nitrogen.
Fig. 4 is a contact angle test chart of the low temperature resistant flexible nano heat insulation material prepared in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without creative efforts, based on the described embodiments of the present invention belong to the protection scope of the present invention.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
As shown in fig. 1, in one aspect, the embodiment of the invention provides a preparation method of a low-temperature-resistant flexible nano heat insulation material, which comprises the following steps:
(1) Uniformly mixing inorganic fibers and organic fibers according to the weight ratio of (65-85) (15-35), and forming a hybrid fiber felt by a mechanical reinforcement method;
(2) Mixing silicate, aminosilane, aldehyde, hexamethylenediamine and alcohol uniformly, stirring at 25-55 ℃ for reaction, and ending the reaction when the pH value of the mixed solution reaches 6.5-7.5 to obtain sol; then mixing the sol and the gel catalyst at room temperature for 2-5 min to obtain a pre-gel solution;
(3) Placing the mixed fiber felt into a pre-gel solution, and soaking for 5-8 min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 5-10 h in a constant temperature environment of 40-60 ℃;
(5) Removing the film coated on the surface of the aged fiber wet felt, and drying to obtain a low-temperature-resistant flexible nano heat-insulating material prefabricated product;
(6) And adhering a steam barrier film with back glue to the surface of the low-temperature-resistant flexible nano heat-insulating material preform through roll forming to form the low-temperature-resistant flexible nano heat-insulating material.
According to the preparation method of the low-temperature-resistant flexible nano heat-insulating material, disclosed by the embodiment of the invention, the low-temperature resistance of a finished product material can be improved by adopting an organic-inorganic blend fiber base material with a certain proportion, and the crystallization embrittlement of a fiber framework structure at a low temperature is avoided; the flexibility in the molding process of the nano material can be improved by introducing the aminosilane, the aldehyde and the hexamethylenediamine in the sol process of the silicon-based aerogel, the crosslinking compactness in the forming process of the nano network structure is enhanced, the adhesive force of the sol and the fiber base material is enhanced, the overall flexibility of the material is increased, the low temperature resistance of the material is further enhanced, and the composite material with the flexibility and the cold transfer isolation is formed.
In some embodiments of the invention, in step (1), the hybrid fiber mat has a density of 120kg/m or less 3 Oxygen index > 32.
In some embodiments of the present invention, in the step (1), the weight ratio of the inorganic fiber to the organic fiber is preferably (75-85): 15-25, and the mixture ratio of the inorganic fiber to the organic fiber is limited, so that the low-temperature brittleness of the heat insulation material is improved, and the heat insulation material has a flame retardant effect.
In some embodiments of the invention, in step (1), the inorganic fibers are glass fibers or basalt fibers having a diameter of 5 to 10 μm and a length of 3 to 10 cm; the organic fiber is any one of nylon (polyamide fiber), polyvinyl chloride fiber, polyurethane fiber, terylene (polyester fiber), polyethylene terephthalate (PET), polybutylene terephthalate (PBT) or polytrimethylene terephthalate (PTT) with the diameter of 5-14 μm and the length of 5-10 cm.
In some embodiments of the invention, in step (2), the weight ratio of silicate, aminosilane, aldehyde, hexamethylenediamine, alcohol is: (50-80): (12-23): (5-18): (2-9): (100-160).
In some embodiments of the invention, in step (2), the silicate is any one of methyl silicate, ethyl silicate, methyltrimethoxysilane, propyltriethoxysilane, or cyclohexyltrimethoxysilane;
and/or the aminosilane is aminoethyltrimethoxy silane or triaminopropyl triethoxy silane;
and/or, the aldehyde is formaldehyde or trimesic aldehyde;
and/or the alcohol is methanol or ethanol.
By introducing aminosilane, aldehyde and hexamethylenediamine in the sol process of the silica-based aerogel, the crosslinking compactness in the sol nano-network structure forming process can be enhanced, so that the silica-based aerogel is more tightly combined with a fiber base material, the overall flexibility of the material is improved, and the low temperature resistance of the material is further enhanced.
In some embodiments of the invention, in step (2), the weight ratio of sol to gel catalyst is 100 (2-8);
further, the gel catalyst is 5wt% -10 wt% ammonia water or sodium hydroxide solution.
In some embodiments of the invention, in step (4), the constant temperature environment is provided by hot water and/or hot nitrogen; by aging in a closed environment, volatilization of the organic solvent in the fiber wet felt can be avoided; and the ageing heat supply mode is optimized, so that the operation safety can be improved.
In some embodiments of the invention, in step (5), the drying is any one of supercritical drying, atmospheric drying, or conduction drying;
further, the process conditions of supercritical drying are as follows: CO 2 The flow rate of the catalyst is 120-260 kg/h, the drying temperature is 45-55 ℃, the drying pressure is 14.5-16.5 MPa, and the drying time is 5-8 h;
the normal pressure drying process conditions are as follows: the temperature of the hot nitrogen is 85-105 ℃ and the flow rate is 30m 3 And/h, the drying time is 10-18 h;
the process conditions of conduction drying are as follows: n-hexane is used as a drying medium, the purity of the medium is 90-98%, the flow rate of the medium is 0.5-1.5 t/h, the temperature of the medium is 70-85 ℃, and the drying time is 8-15 h.
In some embodiments of the present invention, in the step (6), the vapor barrier film with the back adhesive is formed by laminating a metal aluminum foil back adhesive with a thickness of 12-25 wires with any one of PI (polyimide), modified ABS (acrylonitrile butadiene styrene), PTFE (polytetrafluoroethylene), PPO (polyphenylene oxide) and PE (polyethylene) films with a thickness of 5-12 wires.
The embodiment of the invention also provides a low-temperature-resistant flexible nano heat-insulating material, which is prepared by the preparation method.
The features and advantages described above for the preparation method of the low temperature resistant flexible nano heat insulation material are also applicable to the low temperature resistant flexible nano heat insulation material, and are not described herein.
The technical scheme of the invention is further described in detail below with reference to specific examples, wherein the experimental methods without specific conditions are conventional methods and conventional conditions well known in the art.
Example 1
The preparation method of the low-temperature-resistant flexible nano heat-insulating material comprises the following steps:
(1) Uniformly mixing glass fiber and nylon according to a weight ratio of 65:35, and forming the fiber-reinforced nylon fiber with uniform texture and density of 120kg/m by a mechanical reinforcement method 3 A hybrid fiber mat having an oxygen index of 33;
(2) Uniformly mixing methyl silicate, amino ethyl trimethoxy silane, formaldehyde, hexamethylenediamine and methanol according to the weight ratio of 79:12:6:3:160, stirring at 55 ℃ for reaction until the pH value of the mixed solution reaches 6.5, and obtaining sol; then 8wt% ammonia water is prepared as a gel catalyst, and the sol and the gel catalyst are mixed for 2min according to the weight ratio of 100:8 at room temperature to obtain a pre-gel solution;
(3) Quickly placing the hybrid fiber felt into a pre-gel solution, and soaking for 5min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 5 hours in constant-temperature hot water at 60 ℃;
(5) Removing the film coated on the surface of the aged wet fiber felt, and performing supercritical drying (wherein the supercritical drying condition is CO 2 260kg/h, drying temperature 45 ℃, drying pressure 14.5MPa and drying time 5 h) to obtain a low-temperature-resistant flexible nano heat-insulating material prefabricated product;
(6) Cleaning floating glue on the surface of the low-temperature-resistant flexible nano heat-insulating material prefabricated product by using a brush or a dust collector; and meanwhile, a vapor barrier film formed by compounding a metal aluminum foil back adhesive with the thickness of 12 wires and a PE (polyethylene) film with the thickness of 10 wires is selected, and is attached to the surface of a low-temperature-resistant flexible nano heat-insulating material prefabricated product by rolling, so that the low-temperature-resistant flexible nano heat-insulating material is formed.
FIG. 2a is an optical photograph of the low temperature resistant flexible nano heat insulation material prepared in this example; fig. 2b is an optical photograph of the low temperature resistant flexible nano heat insulation material prepared in this example in the bending process after being immersed in liquid nitrogen for 48 hours. As can be seen from fig. 2b, the low temperature-resistant flexible nano heat insulation material prepared by the embodiment has good bending resistance at low temperature, can be bent even after being soaked in liquid nitrogen for 48 hours, and has good low temperature flexibility.
In addition, the low-temperature-resistant flexible nano heat insulation material prepared by the embodiment has good cold insulation performance, and the thermal conductivity at 25 ℃ is 0.015W/(mK); the rebound of the slightly pressed material is obvious, and the slightly pressed material has certain elastic performance; the water contact hydrophobic angle of the water-repellent paint is 135 degrees, and the water-repellent paint has good hydrophobic performance; the material has flame retardant property and oxygen index of 30.
Example 2
The preparation method of the low-temperature-resistant flexible nano heat-insulating material comprises the following steps:
(1) Uniformly mixing basalt fiber and spandex according to a weight ratio of 85:15, and forming a uniform texture with a density of 110kg/m through a mechanical reinforcement method 3 A hybrid fiber mat having an oxygen index of 36;
(2) Uniformly mixing ethyl silicate, trisaminopropyl triethoxysilane, formaldehyde, hexamethylenediamine and ethanol according to the weight ratio of 72:15:8:5:145, stirring at 55 ℃ for reaction, and ending the reaction until the pH value of the mixed solution reaches 7.0 to obtain sol; then preparing 5wt% ammonia water as a gel catalyst, and mixing the sol and the gel catalyst for 4min at room temperature according to a weight ratio of 100:3 to obtain a pre-gel solution;
(3) Quickly placing the hybrid fiber felt into a pre-gel solution, and soaking for 6min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 5 hours in a constant temperature environment of 60 ℃ provided by the combined action of hot water and hot helium;
(5) Removing the film coated on the surface of the aged fiber wet felt, and performing conventional drying (wherein the conventional drying conditions are that n-hexane is used as a drying medium, the medium purity is 98%, the medium flow is 1.5t/h, the medium temperature is 70 ℃ and the drying time is 8 h) to obtain a low-temperature-resistant flexible nano heat-insulating material preform;
(6) Cleaning floating glue on the surface of the low-temperature-resistant flexible nano heat-insulating material prefabricated product by using a brush or a dust collector; and meanwhile, a vapor barrier film formed by compounding a metal aluminum foil back adhesive with the thickness of 12 wires and a PTFE (polytetrafluoroethylene) film with the thickness of 10 wires is selected, and is attached to the surface of a low-temperature-resistant flexible nano heat-insulating material prefabricated product by rolling, so that the low-temperature-resistant flexible nano heat-insulating material is formed.
Fig. 3 is a stress-strain curve diagram of the low-temperature-resistant flexible nano heat insulation material prepared in the embodiment 2 before and after soaking in liquid nitrogen for 48 hours, and as can be seen from the graph, the mechanical strength of the material changes little after soaking in liquid nitrogen, which indicates that the low-temperature-resistant performance of the material is better. In addition, the low-temperature-resistant flexible nano heat insulation material prepared by the embodiment has good cold insulation performance, and the thermal conductivity at 25 ℃ is 0.016W/(mK); the rebound of the slightly pressed material is obvious, and the slightly pressed material has certain elastic performance; and after being soaked in liquid nitrogen for 48 hours, the material is well bent; the contact hydrophobic angle of the heat insulation material with water is 145 degrees, and the heat insulation material has good hydrophobic performance; the material has flame retardant property and oxygen index of 35.
Example 3
The preparation method of the low-temperature-resistant flexible nano heat-insulating material comprises the following steps:
(1) Uniformly mixing glass fiber and terylene according to the weight ratio of 80:20, and forming the uniform-texture density of 120kg/m by a mechanical reinforcement method 3 A hybrid fiber mat having an oxygen index of 35;
(2) Uniformly mixing propyltriethoxysilane, trisaminopropyltriethoxysilane, formaldehyde, hexamethylenediamine and ethanol according to a weight ratio of 67:15:10:8:135, stirring at 45 ℃ for reaction, and ending the reaction until the pH value of the mixed solution reaches 6.5 to obtain sol;
then preparing 5wt% sodium hydroxide solution as a gel catalyst, and mixing the sol and the gel catalyst for 4min at room temperature according to a weight ratio of 100:3 to obtain a pre-gel solution;
(3) Quickly placing the hybrid fiber felt into a pre-gel solution, and soaking for 8 minutes at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 8 hours in a constant temperature environment of 45 ℃ provided by the combined action of hot water and hot helium;
(5) Removing the film coated on the surface of the aged wet fiber felt, and drying under normal pressure (wherein the condition of normal pressure drying is that the temperature of hot nitrogen is 105 ℃ and the flow rate is 30 m) 3 And/h, the drying time is 18 h), and then the low-temperature-resistant flexible nano heat-insulating material prefabricated product is obtained;
(6) Cleaning floating glue on the surface of the low-temperature-resistant flexible nano heat-insulating material prefabricated product by using a brush or a dust collector; and meanwhile, a vapor barrier film formed by compounding a metal aluminum foil back adhesive with the thickness of 18 wires and a PI (polyimide) film with the thickness of 5 wires is selected, and is attached to the surface of a low-temperature-resistant flexible nano heat-insulating material prefabricated product by rolling, so that the low-temperature-resistant flexible nano heat-insulating material is formed.
The low-temperature-resistant flexible nano heat insulation material prepared by the embodiment has good cold insulation performance, and the thermal conductivity at 25 ℃ is 0.016W/(mK); the rebound of the slightly pressed material is obvious, and the slightly pressed material has certain elastic performance; and after being soaked in liquid nitrogen for 48 hours, the material is well bent; the contact hydrophobic angle of the heat insulation material with water is 135 degrees, and the heat insulation material has good hydrophobic performance; and the material has flame retardant property, and the oxygen index is 32.
Example 4
The preparation method of the low-temperature-resistant flexible nano heat-insulating material comprises the following steps:
(1) Uniformly mixing glass fiber and nylon according to a weight ratio of 75:25, and forming a uniform-texture density of 100kg/m by a mechanical reinforcement method 3 A hybrid fiber mat having an oxygen index of 37;
(2) Uniformly mixing methyl silicate, amino ethyl trimethoxy silane, formaldehyde, hexamethylenediamine and methanol according to the weight ratio of 55:23:13:9:110, stirring at 35 ℃ for reaction until the pH value of the mixed solution reaches 7.5, and obtaining sol; then preparing 5wt% sodium hydroxide solution as a gel catalyst, and mixing the sol and the gel catalyst for 5min at room temperature according to the weight ratio of 100:2 to obtain a pre-gel solution;
(3) Quickly placing the hybrid fiber felt into a pre-gel solution, and soaking for 3min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 6 hours in a constant temperature environment of 50 ℃ provided by the combined action of hot water and hot helium;
(5) Removing the film coated on the surface of the aged wet fiber felt, and performing supercritical drying (wherein the supercritical drying condition is CO 2 180kg/h of flow, 45 ℃ of drying temperature, 14.5MPa of drying pressure and 5h of drying time) to obtain a low-temperature-resistant flexible nano heat-insulating material prefabricated product;
(6) Cleaning floating glue on the surface of the low-temperature-resistant flexible nano heat-insulating material prefabricated product by using a brush or a dust collector; and meanwhile, a vapor barrier film formed by compounding a metal aluminum foil back adhesive with the thickness of 15 wires and a PE (polyethylene) film with the thickness of 10 wires is selected, and is attached to the surface of a low-temperature-resistant flexible nano heat-insulating material prefabricated product by rolling, so that the low-temperature-resistant flexible nano heat-insulating material is formed.
The contact angle test is carried out on the low-temperature-resistant flexible nano heat insulation material prepared by the embodiment, and the result is shown in fig. 4, and the heat insulation material prepared by the embodiment has a hydrophobic angle of 141.3 degrees when being contacted with water, which indicates that the heat insulation material has good hydrophobic performance. In addition, the low-temperature-resistant flexible nano heat insulation material prepared by the embodiment has good cold insulation performance, and the thermal conductivity at 25 ℃ is 0.018W/(mK); the rebound of the slightly pressed material is obvious, and the material is well bent and shows better flexibility after being soaked in liquid nitrogen for 48 hours; the material has flame retardant property and oxygen index of 35.
Example 5
The preparation method of the low-temperature-resistant flexible nano heat-insulating material comprises the following steps:
(1) Glass fiber and polytrimethylene terephthalate (PTT) are pressedMixing evenly in a weight ratio of 85:15, and forming the density of 120kg/m with even texture by a mechanical reinforcement method 3 A hybrid fiber mat having an oxygen index of 38;
(2) Uniformly mixing cyclohexyl trimethoxy silane, amino ethyl trimethoxy silane, trimesic aldehyde, hexamethylenediamine and methanol according to the weight ratio of 80:12:5:3:160, stirring at 30 ℃ for reaction, and ending the reaction until the pH value of the mixed solution reaches 6.5 to obtain sol; then preparing 6wt% ammonia water as a gel catalyst, and mixing the sol and the gel catalyst for 3min at room temperature according to the weight ratio of 100:5 to obtain a pre-gel solution;
(3) Quickly placing the hybrid fiber felt into a pre-gel solution, and soaking for 5min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 10 hours in a constant temperature environment of 55 ℃ provided by the combined action of hot water and hot helium;
(5) Removing the film coated on the surface of the aged wet fiber felt, and performing supercritical drying (wherein the supercritical drying condition is CO 2 240kg/h of flow, 55 ℃ of drying temperature, 15.5MPa of drying pressure and 8h of drying time) to obtain a low-temperature-resistant flexible nano heat-insulating material prefabricated product;
(6) Cleaning floating glue on the surface of the low-temperature-resistant flexible nano heat-insulating material prefabricated product by using a brush or a dust collector; and meanwhile, a vapor barrier film formed by compounding a metal aluminum foil back adhesive with the thickness of 20 wires and a PPO (polyphenylene oxide) film with the thickness of 12 wires is selected, and is attached to the surface of a low-temperature-resistant flexible nano heat-insulating material prefabricated product by rolling, so that the low-temperature-resistant flexible nano heat-insulating material is formed.
The low-temperature-resistant flexible nano heat insulation material prepared by the embodiment has good cold insulation performance, and the thermal conductivity at 25 ℃ is 0.014W/(mK); the rebound of the slightly pressed material is obvious, and the slightly pressed material has certain elastic performance; and after being soaked in liquid nitrogen for 48 hours, the material is well bent; the contact hydrophobic angle of the heat insulation material with water is 145 degrees, and the heat insulation material has good hydrophobic performance; and the material has flame retardant property, and the oxygen index is 36.
According to the preparation method of the low-temperature-resistant flexible nano heat-insulating material, the heat-insulating material with good low-temperature resistance and flexibility is prepared by adopting the organic-inorganic hybrid fiber base material and aerogel, the heat conductivity of the material at 25 ℃ is less than or equal to 0.018W/(mK), the material can be applied to a cryogenic working condition of 200 ℃ to-198 ℃, and the problems of insufficient low-temperature resistance, poor construction flexibility, difficult installation and the like of the conventional aerogel composite material are solved; meanwhile, the heat insulation material prepared by the embodiment of the invention has good hydrophobic property, and the hydrophobic angle of the heat insulation material contacted with water is more than or equal to 135 degrees; in the embodiment of the invention, the oxygen index of the prepared heat insulation material is more than or equal to 30 by limiting the mixing ratio of the inorganic fibers and the organic fibers, and the heat insulation material has the characteristic of flame retardance; in addition, the heat insulation material also has the characteristic of being capable of being cut, is easy to construct and is wide in application.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (7)
1. The preparation method of the low-temperature-resistant flexible nano heat-insulating material is characterized by comprising the following steps of:
(1) Uniformly mixing inorganic fibers and organic fibers according to the weight ratio of (65-85) (15-35), and forming a hybrid fiber felt by a mechanical reinforcement method; wherein the inorganic fiber is glass fiber or basalt fiber with the diameter of 5-10 mu m and the length of 3-10 cm; the organic fiber is any one of nylon, chlorlon, spandex, dacron, polyethylene terephthalate, polybutylene terephthalate or polypropylene terephthalate with the diameter of 5-14 mu m and the length of 5-10 cm;
(2) Mixing silicate, aminosilane, aldehyde, hexamethylenediamine and alcohol uniformly, stirring at 25-55 ℃ for reaction, and ending the reaction when the pH value of the mixed solution reaches 6.5-7.5 to obtain sol; then mixing the sol and the gel catalyst at room temperature for 2-5 min to obtain a pre-gel solution; wherein, the weight ratio of silicate, aminosilane, aldehyde, hexamethylenediamine and alcohol is as follows: (50-80): 12-23): 5-18): 2-9): 100-160; the silicate is any one of methyl silicate, ethyl silicate, methyltrimethoxysilane, propyltriethoxysilane or cyclohexyltrimethoxysilane; the aminosilane is aminoethyltrimethoxy silane or triaminopropyl triethoxy silane; the aldehyde is formaldehyde or trimesic aldehyde; the alcohol is methanol or ethanol;
(3) Placing the mixed fiber felt into a pre-gel solution, and soaking for 5-8 min at room temperature to form a fiber wet felt with saturated adsorption gel;
(4) Coating the surface of the fiber wet felt with a sealing film, and aging for 5-10 h in a constant temperature environment of 40-60 ℃;
(5) Removing the film coated on the surface of the aged fiber wet felt, and drying to obtain a low-temperature-resistant flexible nano heat-insulating material prefabricated product;
(6) And adhering a steam barrier film with back glue to the surface of the low-temperature-resistant flexible nano heat-insulating material preform through roll forming to form the low-temperature-resistant flexible nano heat-insulating material.
2. The method for preparing the low-temperature-resistant flexible nano heat-insulating material according to claim 1, wherein in the step (1), the density of the hybrid fiber felt is less than or equal to 120kg/m 3 Oxygen index > 32.
3. The method for preparing the low-temperature-resistant flexible nano heat-insulating material according to claim 1, wherein in the step (2), the weight ratio of the sol to the gel catalyst is 100 (2-8);
further, the gel catalyst is 5-10wt% ammonia water or sodium hydroxide solution.
4. The method for preparing the low-temperature-resistant flexible nano heat-insulating material according to claim 1, wherein in the step (4), the constant-temperature environment is provided by hot water and/or hot nitrogen.
5. The method for preparing the low-temperature-resistant flexible nano heat-insulating material according to claim 1, wherein in the step (5), the drying mode is any one of supercritical drying, normal-pressure drying or conduction drying;
further, the process conditions of the supercritical drying are as follows: CO 2 The flow rate of the catalyst is 120-260 kg/h, the drying temperature is 45-55 ℃, the drying pressure is 14.5-16.5 MPa, and the drying time is 5-8 h;
the normal pressure drying process conditions are as follows: the temperature of the hot nitrogen is 85-105 ℃ and the flow rate is 30m 3 And/h, the drying time is 10-18 h;
the process conditions of the conduction drying are as follows: n-hexane is used as a drying medium, the purity of the medium is 90-98%, the flow rate of the medium is 0.5-1.5 t/h, the temperature of the medium is 70-85 ℃, and the drying time is 8-15 h.
6. The method for preparing the low-temperature-resistant flexible nano heat-insulating material according to claim 1, wherein in the step (6), the steam-insulating film with the back glue is formed by attaching a metal aluminum foil back glue with the thickness of 12-25 wires to any one of PI and modified ABS, PTFE, PPO, PE films with the thickness of 5-12 wires.
7. The low-temperature-resistant flexible nano heat-insulating material is characterized by being prepared by the preparation method of any one of claims 1-6.
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