CN115583829B - Low-thermal-conductivity fiber composite aerogel wet felt and preparation method thereof - Google Patents
Low-thermal-conductivity fiber composite aerogel wet felt and preparation method thereof Download PDFInfo
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- CN115583829B CN115583829B CN202211320347.5A CN202211320347A CN115583829B CN 115583829 B CN115583829 B CN 115583829B CN 202211320347 A CN202211320347 A CN 202211320347A CN 115583829 B CN115583829 B CN 115583829B
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- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
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Abstract
The invention discloses a low-thermal-conductivity fiber composite aerogel wet felt and a preparation method thereof, wherein the wet felt comprises 50-80% of fibers and 20-50% of aerogel by weight percent; the aerogel wet felt has a thermal conductivity of less than or equal to 0.016W/(m.K) at 25 ℃, a thermal conductivity of less than or equal to 0.032W/(m.K) at 300 ℃ and a thermal conductivity of less than or equal to 0.064W/(m.K) at 500 ℃. The preparation method comprises the steps of firstly dispersing fibers to prepare a fiber suspension; conveying the material to a net curtain of non-woven forming equipment, and sequentially carrying out deposition and vacuum water filtering treatment; then spraying sol glue solution, performing gel in a heating tunnel, rolling, and then sending into a soaking aging tank; finally, carrying out supercritical drying to obtain the finished fiber composite aerogel wet felt. The fiber composite aerogel wet felt prepared by the method has excellent compression performance and quite uniform fiber structure. Has the characteristics of low density, no introduction of organic impurities, good compression performance and excellent heat insulation performance. The method has the advantages of simple preparation process and low production cost, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and particularly relates to a fiber composite aerogel wet felt with a low thermal conductivity coefficient and a preparation method thereof.
Background
The fields of new energy, power batteries, construction, industry, transportation and the like need fireproof, heat preservation, heat insulation, cold preservation and other materials, and the demands for materials with high compression resistance and low heat conductivity coefficient are increasing.
SiO 2 Aerogel is a lightweight nano porous amorphous solid material with very excellent heat-proof and heat-insulating properties, and is specialThe nano-pore structure of (2) makes the nano-pore structure have unique properties in heat insulation and is often used as a heat insulation material. However due to SiO 2 The aerogel has the problems of low strength and large brittleness, greatly limits the application range of the aerogel, and needs to be compounded with fiber reinforcement to obtain SiO with certain mechanical strength 2 Aerogel composite material, in order to meet the practical application requirement.
Currently, existing fiber reinforced materials are mainly divided into two categories: fiber needled felt and fiber wet felt. The fiber needled felt has the advantages of simple process, low cost and the like, but because of the transverse and longitudinal through fibers in the needling process, the heat conductivity of the aerogel composite felt is increased, and the heat insulation effect of the aerogel is reduced. When more than two kinds of fibers are used for making the felt, the defect that the fibers are difficult to mix uniformly exists, and the needled felt has low flatness, so that the application of the needled felt in some precision industries is limited. In the preparation process of the fiber wet-process felt, fibers are easy to disperse uniformly in a water phase, the prepared felt body has no penetrating fibers and has higher flatness, but in the felt forming process, a large amount of organic adhesives are used for cementing staggered fibers, so that on one hand, the heat-resistant and heat-insulating capacity of the felt body is influenced, and on the other hand, VOC (volatile organic compounds) exists in a high-temperature scene S The threat of volatilization, and in the process of compounding the wet felt and the aerogel in the traditional process, a large amount of organic adhesive is dissolved out by the supercritical fluid, so that the pipeline is easy to be blocked, and the environmental protection pressure is also caused.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the fiber composite aerogel wet felt with the ultralow heat conductivity coefficient, which has the extremely low heat conductivity coefficient at low temperature and high temperature and good heat insulation capacity.
Furthermore, the invention also provides a preparation method of the aerogel wet felt, which solves the problems that the temperature resistance and the heat insulation capability of the aerogel felt are weakened, and organic substances are dissolved out to block a pipeline and pollute the environment because a large amount of organic adhesives are used for cementing staggered fibers in the felt forming process in the prior art.
In order to achieve the above object, the technical scheme of the present invention is as follows:
the low-thermal-conductivity fiber composite aerogel wet felt comprises 50-80% of fibers and 20-50% of aerogel by weight percent; the aerogel is SiO 2 An aerogel; the aerogel wet felt has a thermal conductivity of less than or equal to 0.016W/(m.K) at 25 ℃, a thermal conductivity of less than or equal to 0.032W/(m.K) at 300 ℃ and a thermal conductivity of less than or equal to 0.064W/(m.K) at 500 ℃.
The low-thermal-conductivity fiber composite aerogel wet felt takes fibers as a framework structure, and SiO (silicon dioxide) 2 Aerogel is an embedded structure. Make full use of SiO 2 The solid heat conduction is reduced by the fine nano skeleton particles of the aerogel, the gas heat conduction is restrained by the nano pore structure, and meanwhile, the radiation heat transfer is reduced by shielding high-temperature near infrared radiation by the inorganic fibers, so that the SiO is realized 2 Aerogel composites still have very low thermal conductivity and high thermal insulation properties at high temperatures.
Further, the volume density of the aerogel wet felt is 120-320kg/m 3 。
Further, the compression ratio of the aerogel wet felt under the condition of 2MPa is 50-80%.
Further, the fiber is one or more of common glass fiber, high silica glass fiber, aluminum silicate fiber, rock wool fiber, basalt fiber, aramid fiber, magnesium silicate fiber, mullite fiber, pre-oxidized fiber, polyimide fiber and carbon fiber.
Further, the fibers are two or more of common glass fibers, high silica glass fibers, aluminum silicate fibers, rock wool fibers, basalt fibers, aramid fibers, magnesium silicate fibers, mullite fibers, pre-oxidized fiber fibers, polyimide fibers and carbon fibers. Due to single fibre reinforced SiO 2 Aerogel heat insulation composite materials have certain defects, such as large diameter and high strength of high silica glass fiber, but high-temperature heat conductivity coefficient and poor infrared shielding property; the aluminum silicate fiber contains infrared reflecting substance Al 2 O 3 、Fe 2 O 3 Etc., the radiation blocking performance is good, but a small amount of slag balls are contained in the radiation blocking performance, so that the heat insulation effect is affected; the rock wool not only contains TiO 2 、Fe 2 O 3 、Al 2 O 3 The infrared reflecting substances are equal, the fiber diameter is small, the solid state and the radiation heat transfer are well inhibited, but the fiber has poor integral formability and poor structural uniformity; the mullite fiber is composed of mullite phase, has the characteristics of good heat insulation effect, high temperature resistance and the like, and is high in price. The fibers are preferably two or more, which makes up for a single fiber-reinforced SiO 2 The aerogel heat insulation composite material has the advantages of uniform structure, moderate cost and the like while having higher heat insulation performance.
Further, the fibers have a length of 1mm to 50mm and a diameter of 1 μm to 20. Mu.m. By adopting the wet process, the fiber is not easy to disperse if the fiber length is too long; if the fiber length is too short, the fiber is not easy to be molded; the fiber length of the present invention is thus controlled within this range.
The preparation method of the low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a suspension: according to the parts by weight, 10000 parts of tap water, 5-100 parts of thickener, 1-5 parts of dispersant and 0.05-0.5 part of defoamer are respectively added into a stirring tank to be uniformly stirred to obtain a mixed solution, and then 10-500 parts of chopped fibers are added and uniformly mixed to obtain a fiber suspension;
(2) And (3) forming a felt blank: delivering the fiber suspension prepared in the step (1) to a forming machine, sequentially depositing, filtering, and dehydrating in vacuum, and then preparing a felt blank on a forming net;
wherein the deposition time is 40-200 s, the filtering time is 1-30 s, the vacuumizing time is 5-15 s, and the vacuum degree during vacuumizing is 350-450 kpa.
(3) Preparing sol: according to the parts by weight, adding 560-720 parts of alcohol solvent, 70-90 parts of deionized water, 1-10 parts of catalyst 1 and 170-195 parts of silicon source into a hydrolysis kettle respectively, and stirring uniformly to obtain hydrolysis liquid; uniformly mixing the hydrolysate with the catalyst 2 according to the mass ratio of 10-30:1 to obtain sol;
(4) Gluing: transferring the felt blank obtained in the step (2) to a sizing net, and uniformly leaching the sol obtained in the step (3) on the felt blank through a sizing device to obtain a sol composite felt blank;
(5) Gel curing: feeding the sol composite felt blank into an oven or a heating tunnel for gelation to obtain a gel felt;
(6) And (5) felt collecting and aging: the gel felt and the lining net are rolled into a cylinder shape by a rolling machine or the gel felt is sliced and stacked into a tool, and then the tool is placed into an aging tank to be soaked in a solvent, heated and aged; the soaking liquid is one of methanol, ethanol and isopropanol, and the water content of the soaking liquid is not more than 10%; the soaking solution and the solvent in the sol are the same substances, so that the introduction of various impurities is avoided, and finally, the gel curing is achieved. The soaking temperature is 50-70 ℃ and the soaking time is 4-24h.
(7) And (5) drying a finished product: transferring the aged gel felt to a supercritical drying kettle, and performing supercritical drying to obtain a finished product. The supercritical drying mode is CO2 supercritical or ethanol supercritical drying. The CO 2 The drying temperature is 55+/-10 ℃; the drying pressure is 14mpa plus or minus 2mpa; the supercritical drying temperature of the ethanol is more than 245 ℃ and the pressure is more than 8mpa.
Further, in the step (1), the thickener is sodium carboxymethyl cellulose, hydroxyethyl cellulose or methyl cellulose;
the dispersing agent is fatty acid polyethylene glycol ester, polyacrylamide, sodium dodecyl sulfate or polyether modified polysiloxane; the defoamer is polydimethylsiloxane. The dispersing agent, the thickening agent and the defoaming agent are all high-cost performance and high-activity agents, so that the cost is lower and the effect is better.
Further, in the step (3),
the alcohol solvent is methanol, ethanol or isopropanol; the catalyst 1 is hydrochloric acid, sulfuric acid, nitric acid, acetic acid or ammonium fluoride; the silicon source is one or more of methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, hexamethyldisilazane, sodium silicate solution or silica sol; the catalyst 2 is ammonia water, sodium hydroxide solution, sodium carbonate solution or sodium bicarbonate solution.
Further, the heating tunnel in the step (5) is formed by heating a hot water coil, heating by microwaves, heating by infrared rays or heating by ultrasonic waves; the average temperature in the oven or the heating tunnel is 25-55 ℃, and the heating time is 1-15min.
Compared with the prior art, the invention has the following beneficial effects:
1. the fiber composite aerogel wet felt with the ultra-low coefficient of thermal conductivity has the advantages of remarkable heat insulation effect, uniform structure, low density, good compression performance and almost no organic material, and can meet the requirements of new energy, power batteries, buildings, industry, transportation and the like on fire prevention, heat preservation, heat insulation, cold preservation and the like.
2. According to the preparation method of the aerogel wet felt, through the aerogel connecting fibers, the influence of the introduction of the organic adhesive in the traditional wet process on heat conduction is avoided, the blockage of the system by the adhesive dissolved in the supercritical drying process is eliminated, the preparation efficiency is greatly improved, and the time cost and the material cost are saved; and unlike needling process, the fiber mat prepared by the process has no transverse and longitudinal penetrating fibers, so that the effect of a thermal bridge is greatly reduced, the aerogel mat has lower heat conductivity, and the heat conductivity at 25 ℃ is stabilized below 0.016W/(m.K). In addition, as the liquid phase is dispersed, the dispersion of different types of fibers in the method is more uniform, the preparation of the fiber felt with low density, light shielding substance and homogeneous fiber structure is facilitated, the thermal conductivity of the high-temperature section is obviously reduced by combining the excellent thermal property of the aerogel, and the aerogel felt with the thermal conductivity of less than or equal to 0.06W/(m.K) at 500 ℃ can be prepared.
3. The invention combines the fiber felting and aerogel composite technology through specific technology adjustment, shortens the preparation period, reduces the manufacturing cost, and ensures that the product has the advantages of low heat conductivity, good heat insulation capacity and the like. Meanwhile, organic adhesives are not needed in the felting process, so that on one hand, the heat-resistant and heat-insulating effects of the wet-process felt can be improved, and on the other hand, the problems of pipeline blockage and environmental protection pressure caused by a large amount of organic adhesives dissolved out by supercritical fluid in the compounding process of the wet-process felt and aerogel can be avoided.
Drawings
FIG. 1 is a schematic representation of a glass fiber composite aerogel wet laid mat product of example 1 of the present invention;
fig. 2 is a graph of raw data of high temperature thermal conductivity of the fiber composite aerogel wet laid mat of the present invention.
Detailed Description
In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Unless otherwise specified, the starting materials are all commercially available.
In the following examples, the measurement methods of the respective parameters were as follows:
(1) The density measurement method comprises the following steps: reference standard GB/T24218 related content execution;
(2) The method for measuring the compression ratio comprises the following steps: reference standard GB/T13480 related content execution;
(3) The method for measuring the heat conductivity coefficient comprises the following steps: reference standards GB/T10294 and GB/T10295 are executed;
(4) The testing method of the heat insulation performance comprises the following steps: reference is made to the standard CSTM00193-2020 related content execution.
Example 1
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a glass fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 50 parts by mass of methyl cellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 2 parts by mass of fatty acid polyethylene glycol ester and 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 200 parts by mass of prepared alkali-free chopped glass fibers are added, and stirring is continued until the fibers are uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 720 parts by mass of absolute methanol, 90 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 190 parts by mass of methyl orthosilicate (TMOS), and stirring at 40 ℃ for 4 hours to obtain a hydrolysis solution;
mixing the hydrolysate with 0.1mol/L aqueous ammonia alcohol solution according to the mass ratio of 10:1 to obtain sol;
(3) Preparing aerogel composite glass fiber felt:
fully soaking the sol prepared in the step (2) into the glass fiber felt blank prepared in the step (1), then transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the temperature of 45 ℃, transferring the felt to an aging kettle, soaking in absolute methanol at the temperature of 55 ℃ for 10h, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet glass fiber mat with the thickness of 10 mm.
A glass fiber composite aerogel wet laid product diagram is shown in fig. 1.
Example 2
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a mixed fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 40 parts by mass of sodium carboxymethylcellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 2 parts by mass of fatty acid polyethylene glycol ester and 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 100 parts by mass of prepared aluminum silicate fiber and 100 parts by mass of alkali-free chopped glass fiber are added successively, and stirring is continued until the fiber is uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 720 parts by mass of absolute methanol, 90 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of methyl orthosilicate (TMOS), 95 parts by mass of methyltrimethoxysilane (MTMS), and stirring at 40 ℃ for 4 hours to obtain a hydrolysate;
mixing the hydrolysate with 0.1mol/L aqueous ammonia alcohol solution according to the mass ratio of 10:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the felt blank prepared in the step (1), transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the temperature of 45 ℃, transferring the felt into an aging kettle, soaking in absolute methanol at the temperature of 55 ℃ for 10h, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet fiber felt with the thickness of 3 mm.
Example 3
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a mixed fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 40 parts by mass of sodium carboxymethylcellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 3 parts by mass of fatty acid polyethylene glycol ester, 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 50 parts by mass of prepared aluminum silicate fiber, 50 parts by mass of basalt chopped fiber and 50 parts by mass of alkali-free chopped glass fiber are sequentially added, and stirring is continued until the fiber is uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 720 parts by mass of absolute methanol, 90 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of TMOS,95 parts by mass of MTMS, and stirring at 40 ℃ for 4 hours to obtain a hydrolysis solution;
mixing the hydrolysate with 0.1mol/L aqueous ammonia alcohol solution according to the mass ratio of 10:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the felt blank prepared in the step (1), then transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the tunnel temperature of 45 ℃, transferring the felt to an aging kettle, and transferring the felt to a dry armor at the temperature of 55 DEG CSoaking in alcohol for 10 hr, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet fiber felt with the thickness of 3 mm.
Example 4
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a mixed fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 40 parts by mass of sodium carboxymethylcellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 2 parts by mass of fatty acid polyethylene glycol ester and 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 100 parts by mass of prepared basalt fiber and 100 parts by mass of alkali-free chopped glass fiber are added successively, and stirring is continued until the fiber is uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 720 parts by mass of absolute methanol, 90 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of TMOS,95 parts by mass of MTMS, and stirring at 40 ℃ for 4 hours to obtain a hydrolysis solution;
mixing the hydrolysate with 0.1mol/L aqueous ammonia alcohol solution according to the mass ratio of 10:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the felt blank prepared in the step (1), transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the temperature of 45 ℃, transferring the felt into an aging kettle, soaking in absolute methanol at the temperature of 55 ℃ for 10h, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet fiber felt with the thickness of 3 mm.
Example 5
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a mixed fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 40 parts by mass of sodium carboxymethylcellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 2 parts by mass of fatty acid polyethylene glycol ester and 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 100 parts by mass of prepared aluminum silicate fiber and 100 parts by mass of alkali-free chopped glass fiber are added successively, and stirring is continued until the fiber is uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 560 parts by mass of absolute ethyl alcohol, 70 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of Tetraethoxysilane (TEOS), 70 parts by mass of Methyltriethoxysilane (MTES), and stirring at 40 ℃ for 10 hours to obtain a hydrolysate;
mixing the hydrolysate with 1mol/L sodium hydroxide solution according to a mass ratio of 30:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the felt blank prepared in the step (1), transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the temperature of 45 ℃, transferring the felt into an aging kettle, soaking in 95 ethanol at the temperature of 65 ℃ for 24h, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet fiber felt with the thickness of 3 mm.
Example 6
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a mixed fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 40 parts by mass of sodium carboxymethylcellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 3 parts by mass of fatty acid polyethylene glycol ester, 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 50 parts by mass of prepared aluminum silicate fiber, 50 parts by mass of basalt chopped fiber and 50 parts by mass of alkali-free chopped glass fiber are sequentially added, and stirring is continued until the fiber is uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 560 parts by mass of absolute ethyl alcohol, 70 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of TEOS,70 parts by mass of MTES, and stirring at 40 ℃ for 10 hours to obtain a hydrolysis solution;
mixing the hydrolysate with 1mol/L sodium hydroxide solution according to a mass ratio of 30:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the felt blank prepared in the step (1), transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the temperature of 45 ℃, transferring the felt into an aging kettle, soaking in 95 ethanol at the temperature of 65 ℃ for 24h, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet fiber felt with the thickness of 3 mm.
Example 7
A preparation method of a low-thermal-conductivity fiber composite aerogel wet felt comprises the following steps:
(1) Preparing a mixed fiber felt blank:
10000 parts by mass of tap water is weighed and injected into a slurry preparation tank, 40 parts by mass of sodium carboxymethylcellulose is added under the condition of slow stirring, stirring is continued until the solution is transparent, then 2 parts by mass of fatty acid polyethylene glycol ester and 0.1 part by mass of defoamer (polydimethylsiloxane) are added and stirred uniformly, then 100 parts by mass of prepared basalt fiber and 100 parts by mass of alkali-free chopped glass fiber are added successively, and stirring is continued until the fiber is uniformly dispersed in water;
molding by a pulp-flowing and shoveling process, controlling flow to be injected into a molding net, and simultaneously carrying out suction filtration on the bottom of a wet felt blank by using a Roots vacuum pump, wherein the vacuum degree is 400kpa, so as to obtain the wet felt blank;
(2) Configuration of sol:
sequentially adding 560 parts by mass of absolute ethyl alcohol, 70 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of TEOS,70 parts by mass of MTES, and stirring at 40 ℃ for 10 hours to obtain a hydrolysis solution;
mixing the hydrolysate with 1mol/L sodium hydroxide solution according to a mass ratio of 30:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the felt blank prepared in the step (1), transferring into a heating tunnel for gelation, passing through the tunnel for 10min at the temperature of 45 ℃, transferring the felt into an aging kettle, soaking in 95 ethanol at the temperature of 65 ℃ for 24h, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite wet fiber felt with the thickness of 3 mm.
Comparative example 8
(1) Preparing a 10mm fiber needled felt;
(2) Configuration of sol:
sequentially adding 560 parts by mass of absolute ethyl alcohol, 70 parts by mass of deionized water and 1 part by mass of concentrated hydrochloric acid into a hydrolysis kettle, uniformly stirring, then adding 100 parts by mass of TEOS,70 parts by mass of MTES, and stirring at 40 ℃ for 10 hours to obtain a hydrolysis solution;
mixing the hydrolysate with 1mol/L sodium hydroxide solution according to a mass ratio of 30:1 to obtain sol;
(3) Aerogel felt preparation:
fully soaking the sol prepared in the step (2) into the fiber needled felt in the step (1), heating for gelation, transferring the felt to an aging kettle, soaking in 95 ethanol at 65 ℃ for 24 hours, and transferring to CO 2 Drying for 10 hours in a supercritical device to obtain the aerogel composite needled fiber felt with the thickness of 10 mm.
Comparative example 9
The preparation method is the same as that of comparative example 8, except that the 10mm fiber needled felt is replaced by a 3mm fiber wet felt, and finally the 3mm thick aerogel composite fiber wet felt is obtained.
Test example 10
The fiber composite aerogel wet mats prepared in examples 1 to 7 were tested for bulk density, compressibility, thermal conductivity, and thermal insulation properties according to the above-described measurement methods, and the results are shown in table 1.
TABLE 1
As can be seen from the results in the table, the fiber composite aerogel wet-process felt prepared by the method provided by the invention has extremely low heat conductivity coefficient at low temperature and high temperature and good heat insulation capacity. The heat conductivity coefficient at 25 ℃ is less than or equal to 0.016W/(m.K), the heat conductivity coefficient at 300 ℃ is less than or equal to 0.032W/(m.K), and the heat conductivity coefficient at 500 ℃ is less than or equal to 0.064W/(m.K). The fiber composite aerogel wet felt prepared by the method has uniform structure; low density of 120-320kg/m 3 (the invention adopts different types of fibers with larger density adjustment space, the embodiment is experimental data of a trial product, and the main fiber is glass fiber); the thickness is 1-10mm and is adjustable; the compression performance is good, and the compression rate under the condition of 2MPa can reach 80 percent; almost no organic material, and has wide application prospect.
Fig. 2 is a graph of raw data of high-temperature heat conduction of the fiber composite aerogel wet-process felt, and it can be seen from fig. 2 that the high-temperature heat conduction coefficient of the aerogel wet-process felt is obviously reduced compared with that of a conventional aerogel felt.
In addition, the method avoids the influence of the introduction of the organic adhesive on heat conduction in the traditional wet process, eliminates the blockage of the system by the adhesive dissolved in the supercritical drying process, and reduces the material cost of raw materials; meanwhile, the links of drying, rolling and uncoiling the base material are reduced, the transportation links from the base material preparation position to the composite felt preparation position are reduced, two different link production lines are combined into one, the preparation efficiency is greatly improved, and the time cost and the material cost are saved. Has the advantages of short preparation route, simple process method, low influence of the manufacturing process on equipment and the like. And unlike needling process, the fiber mat prepared by the process has no transverse and longitudinal penetrating fibers, so that the effect of a thermal bridge is greatly reduced, the aerogel mat has lower heat conductivity, and the heat conductivity at 25 ℃ is stabilized below 0.016W/(m.K). In addition, as the liquid phase is dispersed, the dispersion of different types of fibers in the method is more uniform, the preparation of the fiber felt with low density, light shielding substance and homogeneous fiber structure is facilitated, the thermal conductivity of the high-temperature section is obviously reduced by combining the excellent thermal property of the aerogel, and the aerogel felt with the thermal conductivity of less than or equal to 0.06W/(m.K) at 500 ℃ can be prepared.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the technical solution, and those skilled in the art should understand that modifications and equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the present invention, and all such modifications and equivalents are included in the scope of the claims.
Claims (8)
1. The low-thermal-conductivity fiber composite aerogel wet felt is characterized by comprising 50-80% of fibers and 20-50% of aerogel by weight percent; the aerogel is SiO 2 An aerogel; the aerogel wet felt has a heat conductivity coefficient of less than or equal to 0.016W/(m.K) at 25 ℃, a heat conductivity coefficient of less than or equal to 0.032W/(m.K) at 300 ℃ and a heat conductivity coefficient of less than or equal to 0.064W/(m.K) at 500 ℃;
the preparation method comprises the following steps:
(1) Preparing a suspension: according to the parts by weight, 10000 parts of tap water, 5-100 parts of thickener, 1-5 parts of dispersant and 0.05-0.5 part of defoamer are respectively added into a stirring tank to be uniformly stirred to obtain a mixed solution, and then 10-500 parts of chopped fibers are added and uniformly mixed to obtain a fiber suspension;
(2) And (3) forming a felt blank: delivering the fiber suspension prepared in the step (1) to a forming machine, sequentially depositing, filtering, and dehydrating in vacuum, and then preparing a felt blank on a forming net;
(3) Preparing sol: according to the parts by weight, adding 560-720 parts of alcohol solvent, 70-90 parts of deionized water, 1-10 parts of catalyst 1 and 170-195 parts of silicon source into a hydrolysis kettle respectively, and stirring uniformly to obtain hydrolysis liquid; uniformly mixing the hydrolysate with the catalyst 2 according to the mass ratio of 10-30:1 to obtain sol;
(4) Gluing: transferring the felt blank obtained in the step (2) to a sizing net, and uniformly leaching the sol obtained in the step (3) on the felt blank through a sizing device to obtain a sol composite felt blank;
(5) Gel curing: feeding the sol composite felt blank into an oven or a heating tunnel for gelation to obtain a gel felt;
(6) And (5) felt collecting and aging: the gel felt and the lining net are rolled into a cylinder shape by a rolling machine or the gel felt is sliced and stacked into a tool, and then the tool is placed into an aging tank to be soaked in a solvent, heated and aged;
(7) And (5) drying a finished product: transferring the aged gel felt to a supercritical drying kettle, and performing supercritical drying to obtain a finished product;
the fiber is one or more of common glass fiber, high silica glass fiber, aluminum silicate fiber, rock wool fiber, basalt fiber, aramid fiber, magnesium silicate fiber, mullite fiber, pre-oxidized fiber, polyimide fiber and carbon fiber;
the catalyst 1 is hydrochloric acid, sulfuric acid, nitric acid, acetic acid or ammonium fluoride;
the catalyst 2 is ammonia water, sodium hydroxide solution, sodium carbonate solution or sodium bicarbonate solution.
2. The low thermal conductivity fiber composite aerogel wet blanket of claim 1 wherein the aerogel wet blanket has a bulk density of 120-320kg/m 3 。
3. The low thermal conductivity fiber composite aerogel wet blanket of claim 1 wherein said aerogel wet blanket has a compression of 50-80% at 2 MPa.
4. The low thermal conductivity fiber composite aerogel wet mat of claim 1, wherein the fibers are two or more of common glass fibers, high silica glass fibers, aluminum silicate fibers, rock wool fibers, basalt fibers, aramid fibers, magnesium silicate fibers, mullite fibers, pre-oxidized fiber fibers, polyimide fibers, and carbon fibers.
5. The low thermal conductivity fiber composite aerogel wet laid mat of claim 1, wherein the fibers have a length of 1mm to 50mm and a diameter of 1 μm to 20 μm.
6. The low thermal conductivity fiber composite aerogel wet laid mat of claim 1, wherein in step (1),
the thickener is sodium carboxymethyl cellulose, hydroxyethyl cellulose or methyl cellulose;
the dispersing agent is fatty acid polyethylene glycol ester, polyacrylamide, sodium dodecyl sulfate or polyether modified polysiloxane;
the defoamer is polydimethylsiloxane.
7. The low thermal conductivity fiber composite aerogel wet laid mat of claim 1, wherein in step (3),
the alcohol solvent is methanol, ethanol or isopropanol;
the silicon source is one or more of methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, hexamethyldisilazane, sodium silicate solution or silica sol.
8. The low thermal conductivity fiber composite aerogel wet mat according to claim 1, wherein the heating tunnel in step (5) is hot water coil heating, microwave heating, infrared heating or ultrasonic heating; the average temperature in the oven or the heating tunnel is 25-55 ℃, and the heating time is 1-15min.
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