CN117800752A - Normal-pressure preparation method and application of low-cost carbon aerogel heat insulation material - Google Patents
Normal-pressure preparation method and application of low-cost carbon aerogel heat insulation material Download PDFInfo
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- CN117800752A CN117800752A CN202311844836.5A CN202311844836A CN117800752A CN 117800752 A CN117800752 A CN 117800752A CN 202311844836 A CN202311844836 A CN 202311844836A CN 117800752 A CN117800752 A CN 117800752A
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 6
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 6
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
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- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims description 3
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- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 3
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Abstract
The invention relates to the technical field of ultra-high temperature materials, and particularly discloses a normal pressure preparation method and application of a low-cost carbon aerogel heat insulation material, wherein the method comprises the following steps: s1, preparing an activated waste graphite felt; s2, fully mixing reactants, a solvent and an alkaline catalyst at room temperature, and carrying out addition and polycondensation reaction to obtain phenolic sol; s3, adding a reinforcing agent and a thickening agent into the phenolic sol, and immersing the activated waste graphite felt into the phenolic sol; s4, sealing and preserving at a certain temperature, and performing polymerization reaction; s5, carrying out acid treatment aging and heat aging on the glue; s6, performing solvent replacement and normal-pressure drying; s7, carbonizing to obtain the carbon aerogel heat insulation material. The invention not only can realize recycling of waste graphite felt, but also protects the pore structure of the carbon aerogel, the prepared carbon aerogel heat insulation material has lower heat conductivity coefficient, the reinforcement body is matched with the shrinkage of the aerogel matrix uniformly, the waste graphite felt is not easy to crack and remove slag, the mechanical property is more excellent, and the carbon aerogel heat insulation material has certain compression resistance and bending resistance.
Description
Technical Field
The invention relates to the technical field of ultra-high temperature materials, in particular to a normal pressure preparation method and application of a low-cost carbon aerogel heat insulation material.
Background
The graphite felt is a soft material made of graphite fibers, has good heat resistance and heat conduction performance, and is widely applied to high-temperature processes including a Czochralski single crystal furnace and the like. The graphite felt is mainly composed of graphite fibers, and the graphite fibers are easy to react with oxygen at high temperature to generate oxidation reaction, so that the structure of the graphite fibers is changed. This oxidation reaction results in a decrease in thermal stability and a decrease in thermal conductivity of the graphite felt, thereby affecting the thermal insulation performance and the service life of the graphite felt. The waste graphite felt used in the high-temperature furnace is the graphite felt damaged or failed in the use process, and does not have the functions of original heat preservation, heat insulation, heat conduction, support and the like, and is waste to be treated or disposed. Waste graphite felt may be affected by high temperature, chemical substances and other factors, so that the performance of the waste graphite felt is reduced or damaged, and the waste graphite felt cannot be used any more. For disposal of waste graphite felt, recycling, reuse, safety disposal, and the like are generally considered to reduce the influence on the environment. The specific treatment mode will be selected according to the nature and purpose of the waste graphite felt.
The carbon aerogel has high porosity and high specific surface area (500-1000 m 2 The porous material of/g) has the following advantages: among all aerogel insulation materials, carbon aerogel has the highest use temperature under non-oxidizing atmosphere; carbon aerogels have very low densities, typically in the range of 0.1-0.3g/cm 3 In between, this gives the carbon aerogel light properties and can be used to prepare light materials or composite materials; the carbon aerogel has a lower heat conductivity coefficient, can effectively isolate heat transfer, and has good heat preservation and heat insulation properties; carbon aerogel has good stability under the conventional chemical environment and is not easy to be chemically corroded or oxidized. The advantages lead the carbon aerogel to be widely applied in the fields of aerospace, military equipment, civil heat insulation and the like.
The simple carbon aerogel has a fragile structure, is easy to break or pulverize, and reduces the service life and reliability. Therefore, the heat insulating material is directly applied to the aerospace field, and the problem of mechanical reinforcement of the heat insulating material must be solved. In addition, the shrinkage rate is large in the preparation process of the carbon aerogel, the linear shrinkage rate in the cracking process is more than 20%, and if the reinforcement is compounded with the aerogel matrix for reinforcement, the problem of shrinkage matching between the reinforcement and the matrix becomes a key for solving the reinforcement problem of the carbon aerogel.
Therefore, the development of a carbon aerogel heat insulation felt which can realize recycling of waste graphite felt, has ideal heat insulation performance and excellent mechanical property, has certain compression resistance and bending resistance in the use process, and is consistent and matched with shrinkage of an aerogel matrix to obtain the crack-free carbon aerogel heat insulation felt is needed in the field.
Disclosure of Invention
The invention aims to provide a normal pressure preparation method and application of a low-cost carbon aerogel heat insulation material, which not only realize recycling of waste graphite felt, but also protect the pore structure of the carbon aerogel.
The invention is realized by the following technical scheme:
the normal pressure preparation method of the low-cost carbon aerogel heat insulation material comprises the following steps:
s1, sequentially soaking the waste graphite felt in a hydroxyl-containing polar organic solvent, performing ultrasonic treatment and drying to obtain an activated waste graphite felt;
s2, fully mixing reactants, a solvent and an alkaline catalyst at room temperature, and carrying out addition and polycondensation reaction to obtain phenolic sol;
s3, adding an enhancer and a thickener into the phenolic sol, and immersing the activated waste graphite felt into the phenolic sol to obtain GF/RF sol;
s4, sealing the GF/RF sol and preserving at a certain temperature, and performing polymerization reaction to obtain GF/RF gel;
s5, performing acid treatment aging and thermal aging on the GF/RF gel to obtain GF/RF hydrogel;
s6, performing solvent replacement on the GF/RF hydrogel, and drying at normal pressure to obtain GF/RF aerogel;
s7, carbonizing the GF/RF aerogel to obtain a carbon aerogel heat insulation material;
wherein, steps S1 and S2 are not sequenced.
The waste graphite felt used in the invention is used as a reinforcement of carbon aerogel, and comprises waste graphite felt damaged and failed in a Czochralski single crystal furnace, waste graphite felt damaged and failed in a heat treatment furnace, waste graphite felt damaged and failed in a high temperature furnace, waste graphite felt damaged and failed in a vacuum furnace and the like.
According to the invention, in the process of preparing the carbon aerogel heat insulation material, the waste graphite felt is added as the reinforcing body, and a certain reinforcing agent and a thickening agent are added at the same time, so that the problem that the simple carbon aerogel is fragile in structure and easy to break or pulverize can be solved, and the waste graphite felt serving as the reinforcing body is matched with the shrinkage of the aerogel matrix in a consistent manner, so that the crack-free carbon aerogel heat insulation material can be prepared.
The invention can realize the recycling of waste graphite felt, realize the waste utilization, further realize the reduction of the preparation cost of the carbon aerogel heat insulation material, protect the pore structure of the carbon aerogel, and the prepared carbon aerogel heat insulation material has lower heat conductivity coefficient, the reinforcement is matched with the shrinkage of the aerogel matrix consistently, the waste graphite felt is not easy to crack and remove slag, the mechanical property is more excellent, and the carbon aerogel heat insulation material has certain compression resistance and bending resistance.
Further, in step S1, the polar organic solvent containing hydroxyl group includes alcohol solvents; the soaking temperature is room temperature and the soaking time is 60-120 min.
Further, in the step S1, the ultrasonic frequency is 10-35 kHz; the ultrasonic time is 30-60 min.
Further, in step S1, the drying temperature is 50-70 ℃, and the drying time is 2-3 hours.
Further, in step S2, the reactants include at least one of resorcinol and formaldehyde, melamine and formaldehyde, phenol and furfural, cresol and formaldehyde; the solvent is at least one of water, alcohol organic solvent and ketone organic solvent; the alkaline catalyst is at least one of sodium hydroxide, sodium carbonate, potassium carbonate, calcium hydroxide, magnesium acetate and hexamethylenetetramine.
Further, in step S3, the mass ratio of the phenolic sol to the reinforcing agent is 1: (0.025-0.045).
Further, in step S3, the mass ratio of the phenolic sol to the thickener is 1: (0.06-0.08).
Further, in the step S4, the temperature of sealing and preserving is 60-90 ℃, and the time of sealing and preserving is 24-72 hours.
Further, in step S5, the acid solution used for acid treatment and aging includes at least one of dilute hydrochloric acid, carbonic acid and trifluoroacetic acid, and the solvent used for acid treatment and aging is at least one of acetone, methanol and ethanol; the temperature of heat aging is 50-65 ℃; the heat aging time is 10-36 h.
The application of the carbon aerogel heat insulation material prepared by the normal pressure preparation method is used for preparing an ultrahigh temperature heat insulation product, wherein the ultrahigh temperature heat insulation product comprises a carbon aerogel heat insulation material plate or a carbon aerogel heat insulation material felt.
Compared with the prior art, the invention has the following advantages and beneficial effects:
in the invention, waste graphite felt is added as a reinforcing body in the process of preparing the carbon aerogel heat insulation material, and a certain reinforcing agent and a thickening agent are added at the same time; the method has the advantages that the recycling of waste graphite felt is realized, the waste utilization is realized, the preparation cost of the carbon aerogel heat insulation material is reduced, the pore structure of the carbon aerogel is protected, the heat conductivity coefficient is lower, the reinforcement body is matched with the shrinkage of the aerogel matrix uniformly, the slag is not easy to crack, the mechanical property is more excellent, and certain compression resistance and bending resistance are realized. The invention greatly reduces the production cost by reusing the waste graphite felt, realizes energy conservation and emission reduction by adopting the normal pressure drying technology, is safe and reliable, is suitable for industrial production, and can meet the application of various building scenes.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be described in further detail with reference to the following examples, which are illustrative embodiments of the present invention and the description thereof are intended to be illustrative of the present invention and not limiting of the present invention, and the examples described below are some, but not all, examples of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: no such specific details are necessary to practice the invention. In other instances, well-known structures, materials, or methods have not been described in detail in order to avoid obscuring the present invention. Materials, instruments, reagents and the like used in the following examples are commercially available unless otherwise specified. The technical means used in the examples, unless otherwise specified, are conventional means well known to those skilled in the art.
In order to realize recycling of waste graphite felt and solve the problem of mechanical enhancement of pure carbon aerogel, the embodiment provides a normal pressure preparation method of a low-cost carbon aerogel heat insulation material, which comprises the following steps:
s1, sequentially soaking the waste Graphite Felt (GF) in a hydroxyl-containing polar organic solvent, performing ultrasonic treatment and drying to obtain the activated waste graphite felt.
Wherein the hydroxyl-containing polar organic solvent comprises an alcoholic solvent, preferably anhydrous methanol; the mass ratio of the waste graphite felt to the hydroxyl-containing polar organic solvent is 1: (20-100), preferably 1:50.
the soaking temperature is room temperature; the soaking time is 60-120 min; the frequency of the ultrasonic wave is 10-35 kHz; the ultrasonic time is 30-60 min; the drying temperature is 50-70 ℃; the drying time is 2-3 h.
S2, fully mixing the reactant, the solvent and the alkaline catalyst at room temperature, and carrying out addition and polycondensation reaction to obtain the phenolic aldehyde (RF) sol.
Wherein the reactants comprise at least one of resorcinol and formaldehyde, melamine and formaldehyde, phenol and furfural, cresol and formaldehyde; preferably, the reactant is a mixture of resorcinol and formaldehyde in a molar ratio of 1:2.5.
the solvent is at least one of water, alcohol organic solvent and ketone organic solvent, preferably, the alcohol organic solvent is methanol and the ketone organic solvent is acetone; the alkaline catalyst comprises sodium hydroxide (NaOH), sodium carbonate (Na 2 CO 3 ) Potassium carbonate (K) 2 CO 3 ) Calcium hydroxide (Ca (OH) 2 ) At least one of magnesium acetate and hexamethylenetetramine, preferably sodium carbonate.
Wherein the mol ratio of the solvent to the reactant is (30-100): 1, preferably 60:1, the mol ratio of the reactant to the alkaline catalyst is (300-500): 1, preferably 450:1.
the mixing temperature is room temperature, which in this example is generally 20 to 35 ℃. The reaction time is 20-40 min, and the stirring speed is 1000-2500 rpm/min.
S3, adding the reinforcing agent and the thickening agent into the phenolic sol, and immersing the activated waste graphite felt into the phenolic sol to obtain the GF/RF sol.
Wherein the reinforcing agent comprises N, N-dimethylformamide; preferably, the mass ratio of the phenolic (RF) sol to the reinforcing agent is 1: (0.025 to 0.045), more preferably 1:0.035.
wherein the reinforcing agent comprises methyl cellulose; preferably, the mass ratio of the phenolic (RF) sol to the thickener is 1: (0.06 to 0.08), more preferably 1:0.07.
immersing the activated waste graphite felt into phenolic sol to obtain GF/RF sol. The water absorption of the graphite felt is constant, so that the addition of the activated waste graphite felt is sufficient to prepare GF/RF sol
And S4, sealing the GF/RF sol and preserving at a certain temperature, and performing polymerization reaction to obtain the GF/RF gel.
Wherein, the sealing and preserving time is 24-72 h, preferably 28-40 h; the temperature for sealing preservation is 60-90 ℃, preferably 85 ℃.
And S5, performing acid treatment aging and thermal aging on the GF/RF gel to obtain the GF/RF hydrogel.
Wherein the acid solution adopted by the acid treatment aging comprises at least one of dilute hydrochloric acid, carbonic acid and trifluoroacetic acid, and the solvent adopted by the acid treatment aging is at least one of acetone, methanol and ethanol.
Wherein the temperature of the heat aging is 50-65 ℃, preferably 60-65 ℃; the heat aging time is 10 to 36 hours, preferably 20 to 30 hours.
S6, performing solvent replacement on the GF/RF hydrogel, and repeatedly replacing the liquid with the polar organic solvent for 4 processes, and drying at normal pressure to obtain the GF/RF aerogel.
Wherein, when the solvent replacement is performed by using a polar organic solvent, the time of the solvent replacement is 2-6 hours, preferably 5 hours; the temperature of the displacement is 50-65 ℃, preferably 60 ℃. The polar organic solvent may be an alcoholic solvent, preferably methanol.
Wherein, the method of normal pressure drying is a normal pressure grading drying method, and is preferably drying at 55-65 ℃, 75-85 ℃, 95-105 ℃, 115-125 ℃ and 155-165 ℃ in sequence, and the drying time of each stage is 2-5 h.
And S7, carbonizing the GF/RF aerogel to obtain the carbon aerogel heat insulation material.
The carbonization process is to put a GF/RF aerogel sample into a vacuum furnace, vacuumize to below 100Pa, heat to 150 ℃ from room temperature at a heating rate of 4 ℃/min, keep 150 ℃ for continuous vacuumization for 15min, keep vacuum to heat to 1100 ℃ at a heating rate of 2 ℃/min and keep the temperature constant for 4h, and then gradually cool to room temperature to obtain the carbon aerogel heat insulation material.
The carbon aerogel heat insulation material prepared by the embodiment can be used for preparing an ultrahigh temperature heat insulation product, wherein the ultrahigh temperature heat insulation product comprises a carbon aerogel heat insulation material plate or a carbon aerogel heat insulation material felt.
In the embodiment, in the process of preparing the carbon aerogel heat insulation material, waste graphite felt is added as a reinforcing body, and a certain reinforcing agent and a thickening agent are added at the same time; the method has the advantages that the recycling of waste graphite felt is realized, the waste utilization is realized, the preparation cost of the carbon aerogel heat insulation material is reduced, the pore structure of the carbon aerogel is protected, the heat conductivity coefficient is lower, the reinforcement body is matched with the shrinkage of the aerogel matrix uniformly, the slag is not easy to crack, the mechanical property is more excellent, and certain compression resistance and bending resistance are realized. The invention greatly reduces the production cost by reusing the waste graphite felt, realizes energy conservation and emission reduction by adopting the normal pressure drying technology, is safe and reliable, is suitable for industrial production, and can meet the application of various building scenes.
The technical scheme of this embodiment is further described by the following specific examples.
Example 1:
the normal pressure preparation method of the low-cost carbon aerogel heat insulation material comprises the following steps:
(1) Under the condition of room temperature, the waste Graphite Felt (GF) is soaked in absolute methanol for 60min, and the mass ratio of the waste graphite felt to the absolute methanol is 1:50; then carrying out ultrasonic treatment, wherein the ultrasonic frequency is 30kHz, the ultrasonic time is 30min, transferring the materials into an oven after ultrasonic treatment, and drying for 3h at the temperature of 70 ℃ to obtain activated waste graphite felt;
(2) Resorcinol, formaldehyde, water and sodium carbonate (Na 2 CO 3 ) According to 1:2.5:60:2.2X10 -3 Mixing and stirring the mixture in a molar ratio of (2) at room temperature for 25min at a rotating speed of 2000rpm to prepare phenolic aldehyde (RF) sol;
(3) The phenolic (RF) sol obtained in step (2), reinforcing agent (N, N-dimethylformamide) and thickener (methylcellulose) are mixed according to a ratio of 1:0.035: mixing the materials according to the mass ratio of 0.07, stirring for 3min to uniformity at a rotating speed of 2000rpm, immersing the activated waste graphite felt prepared in the step (a 1) into the sol to obtain GF/RF sol, and sealing and preserving for 36h at 85 ℃; the prepared gel has a molar ratio of 1: preparing 1000 hydrochloric acid and a methanol solvent into a dilute acid solution for acid aging treatment, and simultaneously transferring the materials after sealed preservation into a 60 ℃ oven for heat aging for 30 hours to obtain GF/RF hydrogel; immersing GF/RF hydrogel in absolute methanol at 60 ℃ for solvent replacement for 5 hours, and repeating the liquid replacement for 4 procedures to finish the solvent replacement; drying the replaced materials at the temperature of 60 ℃, 80 ℃, 100 ℃, 120 ℃ and 160 ℃ for 2 hours at each stage to obtain GF/RF aerogel; and (3) placing the GF/RF aerogel into a vacuum furnace, vacuumizing to below 100Pa, heating to 150 ℃ from room temperature at a heating rate of 4 ℃/min, keeping the temperature at 150 ℃ for continuously vacuumizing for 15min, keeping the vacuum, heating to 1100 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 4h, and gradually cooling to the room temperature to obtain the carbon aerogel thermal insulation board.
Example 2:
this embodiment is based on embodiment 1, and differs from embodiment 1 in that:
the amount of enhancer (N, N-dimethylformamide) used in step (3) varies, in particular:
the phenolic (RF) sol, reinforcing agent (N, N-dimethylformamide) and thickener (methylcellulose) were mixed according to a ratio of 1:0.01: mixing at a mass ratio of 0.07.
Example 3:
this embodiment is based on embodiment 1, and differs from embodiment 1 in that:
the amount of enhancer (N, N-dimethylformamide) used in step (3) varies, in particular:
the phenolic (RF) sol, reinforcing agent (N, N-dimethylformamide) and thickener (methylcellulose) were mixed according to a ratio of 1:0.05: mixing at a mass ratio of 0.07.
Example 4:
this embodiment is based on embodiment 1, and differs from embodiment 1 in that:
the amount of thickener (methylcellulose) used in step (3) varies, in particular:
the phenolic (RF) sol, reinforcing agent (N, N-dimethylformamide) and thickener (methylcellulose) were mixed according to a ratio of 1:0.035: mixing at a mass ratio of 0.05.
Example 5:
this embodiment is based on embodiment 1, and differs from embodiment 1 in that:
the amount of thickener (methylcellulose) used in step (3) varies, in particular:
the phenolic (RF) sol, reinforcing agent (N, N-dimethylformamide) and thickener (methylcellulose) were mixed according to a ratio of 1:0.035: mixing in a mass ratio of 0.1.
Comparative example 1:
this comparative example is based on example 1, and differs from example 1 in that: the reinforcement changes the waste graphite felt into a good graphite felt.
Comparative example 2:
this comparative example is based on example 1, and differs from example 1 in that: the waste graphite felt is not subjected to an activation treatment.
Comparative example 3:
this comparative example is based on example 1, and differs from example 1 in that: the reinforcement changes the waste graphite felt into a good graphite felt and is not subjected to an activation treatment.
Comparative example 4:
only the waste graphite felt itself, without any treatment.
Comparative example 5:
only the good graphite felt itself, without any treatment.
Comparative example 6:
the preparation method of the carbon aerogel material comprises the following steps:
(1) Pretreatment of resin: dissolving resin with isopropanol at 50-60 ℃, wherein the molar ratio of the resin to the isopropanol is 1:6;
(2) Resorcinol, formaldehyde, solvent (water) and basic catalyst (Na 2 CO 3 ) According to 1:0.4:60: 2.2X10 -3 The mixture is fully stirred for 30min at the room temperature at 2000rpm/min to prepare mixed hydrogel;
(3) The resin treated in the step (1), the reinforcing agent (N, N-dimethylformamide) and the hydrogel prepared in the step (2) are mixed according to the following steps of 1:0.03: mixing uniformly in a mass ratio of 100, and sealing and preserving for 35 hours at 85 ℃; the prepared gel has a molar ratio of 1:1000 hydrochloric acid and a methanol solvent are prepared into a dilute acid solution for acid aging treatment, and the materials after sealed preservation are transferred into a 60 ℃ oven for heat aging for 30 hours; immersing the aged material in absolute methanol at 60 ℃ for solvent replacement for 5 hours, and repeating the liquid replacement for 4 processes to finish the solvent replacement; drying the replaced materials at the temperature of 60 ℃, 80 ℃, 100 ℃, 120 ℃ and 160 ℃ for 2 hours at each stage to prepare the RF aerogel material; placing the RF aerogel into a vacuum furnace, vacuumizing to below 100Pa, heating to 150 ℃ from room temperature at a heating rate of 4 ℃/min, keeping 150 ℃ for continuously vacuumizing for 15min, keeping the vacuum, heating to 1100 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 4h, and gradually cooling to room temperature to obtain the carbon aerogel.
Performance comparison:
the appearance, density, thermal conductivity, mechanical properties and electromagnetic shielding effectiveness of the products prepared in the above examples and comparative examples are shown in Table 1.
The heat conductivity coefficient is measured by a heat conductivity coefficient measuring instrument, and the testing method refers to GB/T10295-2008 heat flow measuring method for measuring steady-state thermal resistance and related characteristics of insulating materials.
The compression strength is tested by adopting an electronic universal tester, and the testing method refers to GB/T13480-2014, measurement of compression performance of heat insulation products for buildings.
The bending strength is tested by an electronic universal tester, and the testing method is referred to GB/T33001-2016 'determination of bending properties of heat insulation products for buildings'.
TABLE 1
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The normal pressure preparation method of the low-cost carbon aerogel heat insulation material is characterized by comprising the following steps of:
s1, sequentially soaking the waste graphite felt in a hydroxyl-containing polar organic solvent, performing ultrasonic treatment and drying to obtain an activated waste graphite felt;
s2, fully mixing reactants, a solvent and an alkaline catalyst at room temperature, and carrying out addition and polycondensation reaction to obtain phenolic sol;
s3, adding an enhancer and a thickener into the phenolic sol, and immersing the activated waste graphite felt into the phenolic sol to obtain GF/RF sol;
s4, sealing the GF/RF sol and preserving at a certain temperature, and performing polymerization reaction to obtain GF/RF gel;
s5, performing acid treatment aging and thermal aging on the GF/RF gel to obtain GF/RF hydrogel;
s6, performing solvent replacement on the GF/RF hydrogel, and drying at normal pressure to obtain GF/RF aerogel;
s7, carbonizing the GF/RF aerogel to obtain a carbon aerogel heat insulation material;
wherein, steps S1 and S2 are not sequenced.
2. The method for preparing a low-cost aerogel thermal insulation material under normal pressure according to claim 1, wherein in step S1, the polar organic solvent containing hydroxyl group comprises an alcohol solvent; the soaking temperature is room temperature and the soaking time is 60-120 min.
3. The method for preparing the low-cost carbon aerogel heat insulation material under normal pressure according to claim 1, wherein in the step S1, the ultrasonic frequency is 10-35 kHz; the ultrasonic time is 30-60 min.
4. The method for preparing a low-cost aerogel thermal insulation material under normal pressure according to claim 1, wherein in the step S1, the drying temperature is 50-70 ℃, and the drying time is 2-3 hours.
5. The method for preparing a low-cost carbon aerogel thermal insulation material according to claim 1, wherein in step S2, the reactants include at least one of resorcinol and formaldehyde, melamine and formaldehyde, phenol and furfural, cresol and formaldehyde; the solvent is at least one of water, alcohol organic solvent and ketone organic solvent; the alkaline catalyst is at least one of sodium hydroxide, sodium carbonate, potassium carbonate, calcium hydroxide, magnesium acetate and hexamethylenetetramine.
6. The method for preparing the low-cost carbon aerogel heat insulation material under normal pressure according to claim 1, wherein in the step S3, the mass ratio of the phenolic sol to the reinforcing agent is 1: (0.025-0.045).
7. The method for preparing the low-cost carbon aerogel heat insulation material under normal pressure according to claim 1, wherein in the step S3, the mass ratio of the phenolic sol to the thickener is 1: (0.06-0.08).
8. The method for preparing the low-cost carbon aerogel heat insulation material under normal pressure according to claim 1, wherein in the step S4, the temperature of sealing and preserving is 60-90 ℃, and the time of sealing and preserving is 24-72 h.
9. The method for preparing the low-cost carbon aerogel heat insulation material under normal pressure according to claim 1, wherein in the step S5, the acid solution adopted by the acid treatment aging comprises at least one of dilute hydrochloric acid, carbonic acid and trifluoroacetic acid, and the solvent adopted by the acid treatment aging is at least one of acetone, methanol and ethanol; the temperature of heat aging is 50-65 ℃; the heat aging time is 10-36 h.
10. Use of the carbon aerogel insulation material prepared by the atmospheric pressure preparation method according to claim 9 for preparing an ultra-high temperature insulation product.
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