CN114717688A - Graphene aerogel fiber, graphene aerogel thermal insulation flocculus and preparation method thereof - Google Patents
Graphene aerogel fiber, graphene aerogel thermal insulation flocculus and preparation method thereof Download PDFInfo
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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Abstract
The invention discloses a graphene aerogel fiber, a graphene aerogel thermal insulation flocculus and a preparation method thereof, and belongs to the technical field of graphene thermal insulation materials. Which comprises the following steps: oxidizing the flake graphite powder to prepare graphene oxide liquid crystal, and performing wet spinning, reduction and supercritical carbon dioxide drying treatment to obtain the graphene aerogel fiber. The graphene aerogel fiber has excellent far infrared absorption and emission capability, can absorb infrared rays emitted by a human body, improve temperature, avoid heat loss, absorb infrared rays in sunlight and improve heat preservation performance; the fiber material has the advantages of low density, ultrahigh specific surface area, high gas heat conduction inhibition efficiency and low heat conductivity.
Description
Technical Field
The invention relates to the technical field of graphene thermal insulation materials, in particular to graphene aerogel fibers, a graphene aerogel thermal insulation flocculus and a preparation method thereof.
Background
The heat insulating material has wide application range, and the material can not be separated from advanced aerospace to daily building household appliances. In recent years, with the increase of energy consumption and the advance of energy conservation and emission reduction, the requirement on the heat insulation performance of materials is increasingly improved, and the improvement of the heat insulation efficiency gradually becomes one of the hot spots of research.
The heat conduction mode of the material mainly comprises three modes of solid heat conduction, gaseous heat conduction and radiation heat conduction. At present, most of heat insulation materials can effectively inhibit solid heat conduction and radiation heat conduction, but gaseous heat conduction is difficult to effectively inhibit, namely, the vacuum heat insulation material can effectively inhibit gaseous heat conduction, but has high density, limited service life and low inhibition efficiency. In these materials, the ratio of the gaseous thermal conductivity to the total thermal conductivity can even reach more than 50%, therefore, reducing the gaseous thermal conductivity is the key to improve the performance of the heat insulation material, however, how to improve the inhibition efficiency of the gaseous thermal conductivity is the main problem facing the current heat insulation material research. Gas heat conduction is the primary means of gaseous heat conduction, transferring heat primarily through gas molecular collisions. Therefore, to suppress gas heat conduction, it is necessary to sufficiently separate gas molecules. Most of the existing heat insulation materials cannot effectively prevent gas molecules from colliding due to large aperture or large through hole structure, so that the gas heat conduction is serious, and the problem of low gas heat conduction inhibition efficiency exists.
Disclosure of Invention
The invention aims to provide graphene aerogel fibers, a graphene aerogel thermal insulation flocculus and a preparation method thereof, and aims to solve the problems that gas heat conduction is serious and gas heat conduction inhibition efficiency is low due to the fact that most of existing thermal insulation materials cannot effectively prevent gas molecules from colliding because of large aperture or large through hole structures.
The technical scheme for solving the technical problems is as follows:
a preparation method of graphene aerogel fibers comprises the following steps:
adding the flake graphite powder into a pre-oxidation treatment solution at the temperature of 60-85 ℃ to react for 4-6 h, adding water into a reaction system for the first time in an ice water bath to cool, standing overnight, performing suction filtration, and naturally drying to obtain pre-oxidized graphite powder; wherein the concentration of the flake graphite powder in the pre-oxidation treatment liquid is 7-17 g/mL;
adding pre-oxidized graphite powder into concentrated sulfuric acid with the mass fraction of 96-98% while stirring to prepare a reaction solution with the concentration of 2-5 g/mL, adding potassium permanganate in batches, controlling the temperature at 30-40 ℃, and stirring for reaction for 1-4 hours; adding water for cooling in an ice water bath, stirring for 2-5 hours, adding hydrogen peroxide until the color of the solution turns yellow, standing overnight, pouring out the supernatant, adding dilute hydrochloric acid with the mass fraction of 3-7%, stirring and mixing, and standing, filtering and cleaning to obtain a concentrated graphene oxide solution;
carrying out centrifugal separation on a graphene oxide solution to obtain graphene oxide liquid crystal with the concentration of 10-20 mg/mL, injecting the graphene oxide liquid crystal into a coagulating bath, carrying out wet spinning to obtain a graphene oxide gel fiber aggregate, adding L-ascorbic acid with the concentration of 5-15% and a chitosan acetic acid solution with the concentration of 1-5 wt%, carrying out reduction treatment at the temperature of 45-55 ℃ for 8-15 h to obtain graphene hydrogel fibers, and drying the graphene hydrogel fibers by supercritical carbon dioxide to obtain the graphene aerogel fibers.
In the present invention, the graphene oxide liquid crystal may be injected into a zinc nitrate coagulation bath, a calcium chloride coagulation bath, or the like.
Further, in the preparation method of the graphene aerogel fiber, the preparation of the pre-oxidation treatment liquid includes: heating concentrated sulfuric acid with the mass fraction of 96-98% in an oil bath at the temperature of 80-95 ℃, and slowly adding potassium persulfate and phosphorus pentoxide respectively and dissolving;
in the pre-oxidation treatment liquid, the concentration of potassium persulfate is 5-17 g/mL, and the concentration of phosphorus pentoxide is 5-15 g/mL.
Further, in the preparation method of the graphene aerogel fiber, the first water adding and cooling operation is as follows: slowly dripping water which is 0.5-1.5 times of the volume of the preoxidation treatment solution into the reaction system, and then adding water which is 5-12 times of the volume of the preoxidation treatment solution once.
Further, in the preparation method of the graphene aerogel fiber, a microporous filter membrane is adopted for suction filtration.
Further, in the preparation method of the graphene aerogel fiber, the mass ratio of the potassium permanganate to the pre-oxidized graphite powder is as follows: (2-5) 1; and equally dividing the potassium permanganate into 4-5 batches, and adding the potassium permanganate into the mixture at intervals of 8-10 min in each batch.
Further, in the preparation method of the graphene aerogel fiber, the operation of centrifuging the graphene oxide solution is as follows: rotating at 4000-5000 rpm for 5-15 min; then, the rotation speed is 10000-12000 r/min, and the time is 25-35 min.
The invention also provides the graphene aerogel fiber prepared by the preparation method of the graphene aerogel fiber.
The invention also provides a graphene aerogel thermal insulation flocculus which is mainly prepared from the following raw materials in parts by weight: the graphene aerogel fiber comprises a flocculus fiber and the graphene aerogel fiber, wherein the addition amount of the graphene aerogel fiber is 3-8% of the mass of the flocculus fiber.
The invention also provides a preparation method of the graphene aerogel thermal insulation flocculus, which comprises the following steps: and uniformly mixing the flocculus fibers and the graphene aerogel fibers to prepare the graphene aerogel thermal insulation flocculus.
The invention has the following beneficial effects:
1. the graphene aerogel fiber has excellent far infrared absorption and emission capability, can absorb infrared rays emitted by a human body, improve temperature, avoid heat loss, absorb infrared rays in sunlight and improve heat preservation performance; the fiber material has the advantages of low density, ultrahigh specific surface area, high gas heat conduction inhibition efficiency and low heat conductivity.
2. According to the preparation method of the graphene aerogel fiber, the advantages of low density and high specific strength of the graphene aerogel are utilized, but the problem of high thermal conductivity still exists, mainly because the solid thermal conductivity of the graphene aerogel is high due to high thermal conductivity of graphene, and the gaseous thermal conductivity of the graphene aerogel is high due to large pore diameter of the graphene aerogel. Therefore, in the preparation process, by the mode of preparing the graphene oxide and reducing the graphene oxide again, the method of introducing defects and hybrid atoms and reducing the aperture by adding chitosan in the preparation process of the graphene oxide is expected to reduce the solid thermal conductivity and the gaseous thermal conductivity of the graphene aerogel, so that the graphene aerogel thermal insulation material with low density, high gas thermal conduction inhibition efficiency and low thermal conductivity is prepared, and the purposes of improving the thermal insulation efficiency and reducing the density of the thermal insulation material are achieved.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
the preparation method of the graphene aerogel fiber of the embodiment includes the following steps:
(1) preparing a pretreatment solution: heating concentrated sulfuric acid with the mass fraction of 96% in an oil bath at the temperature of 80-95 ℃, and slowly adding potassium persulfate and phosphorus pentoxide respectively and dissolving;
in the pre-oxidation treatment liquid, the concentration of potassium persulfate was 5g/mL, and the concentration of phosphorus pentoxide was 5 g/mL.
(2) Preparation of pre-oxidized graphite powder
Adding flake graphite powder into a pre-oxidation treatment liquid at 60 ℃ for reaction for 4 hours, slowly dripping water which is 0.5 time of the volume of the pre-oxidation treatment liquid into a reaction system in an ice water bath, then adding water which is 5 times of the volume of the pre-oxidation treatment liquid for the first time, adding water for cooling, standing overnight, performing suction filtration through a microporous filter membrane, and naturally drying to obtain pre-oxidation graphite powder; wherein the concentration of the flake graphite powder in the pre-oxidation treatment liquid is 7 g/mL;
(3) preparation of graphene oxide solution
Adding pre-oxidized graphite powder into concentrated sulfuric acid with the mass fraction of 97% under stirring to prepare a reaction solution with the concentration of 2g/mL, wherein the mass ratio of the potassium permanganate to the pre-oxidized graphite powder is as follows: 2:1, equally dividing the potassium permanganate into 4 batches, adding the potassium permanganate into the potassium permanganate at intervals of 8min every batch, controlling the temperature to be 30 ℃, and stirring to react for 1 h; adding water for cooling in an ice water bath, stirring for 2 hours, adding hydrogen peroxide until the color of the solution turns yellow, standing overnight, pouring out the supernatant, adding dilute hydrochloric acid with the mass fraction of 3%, stirring and mixing, standing, filtering and cleaning to obtain a concentrated graphene oxide solution;
(4) preparation of graphene aerogel
The graphene oxide solution is rotated at the rotating speed of 4000 revolutions per minute for 5 min; and then carrying out centrifugal separation at a rotation speed of 100000 r/min for 25min to obtain graphene oxide liquid crystal with the concentration of 10mg/mL, injecting the graphene oxide liquid crystal into a zinc nitrate solidification bath, carrying out wet spinning to obtain a graphene oxide gel fiber aggregate, adding L-ascorbic acid with the concentration of 5% and a chitosan acetic acid solution with the concentration of 1 wt%, carrying out reduction treatment at the temperature of 45 ℃ for 8h to obtain graphene hydrogel fiber, and drying the graphene hydrogel fiber by supercritical carbon dioxide to obtain the graphene aerogel fiber.
Example 2:
the preparation method of the graphene aerogel fiber of the embodiment includes the following steps:
(1) preparing a pretreatment solution: heating concentrated sulfuric acid with the mass fraction of 97% in an oil bath at 86 ℃, and slowly adding potassium persulfate and phosphorus pentoxide respectively and dissolving;
in the pre-oxidation treatment liquid, the concentration of potassium persulfate was 12g/mL, and the concentration of phosphorus pentoxide was 8 g/mL.
(2) Preparation of pre-oxidized graphite powder
Adding flake graphite powder into a pre-oxidation treatment liquid at 72 ℃ for reaction for 5 hours, slowly dripping water of which the volume is 1 time of that of the pre-oxidation treatment liquid into a reaction system in an ice water bath, then adding water of which the volume is 7 times of that of the pre-oxidation treatment liquid for one time, adding water for the first time for cooling, standing overnight, performing suction filtration through a microporous filter membrane, and naturally drying to obtain pre-oxidation graphite powder; wherein the concentration of the crystalline flake graphite powder in the pre-oxidation treatment liquid is 12 g/mL;
(3) preparation of graphene oxide solution
Adding pre-oxidized graphite powder into concentrated sulfuric acid with the mass fraction of 97% under stirring to prepare a reaction solution with the concentration of 3.7g/mL, wherein the mass ratio of the potassium permanganate to the pre-oxidized graphite powder is as follows: 3.5:1, equally dividing the potassium permanganate into 4 batches, adding the potassium permanganate at intervals of 10min for each batch, controlling the temperature at 35 ℃, and stirring to react for 2.5 h; adding water in an ice water bath for cooling, stirring for 3.5 hours, adding hydrogen peroxide until the color of the solution turns yellow, standing overnight, pouring out supernatant, adding dilute hydrochloric acid with the mass fraction of 5%, stirring and mixing, standing, filtering and cleaning to obtain a concentrated graphene oxide solution;
(3) preparation of graphene aerogel
The graphene oxide solution is rotated at a speed of 4700 r/min for 8 min; and then carrying out centrifugal separation at the rotating speed of 11000 r/min for 27min to obtain graphene oxide liquid crystal with the concentration of 13mg/mL, injecting the graphene oxide liquid crystal into a zinc nitrate coagulating bath, carrying out wet spinning to obtain a graphene oxide gel fiber aggregate, adding L-ascorbic acid with the concentration of 8% and a chitosan acetic acid solution with the concentration of 3.5 wt%, carrying out reduction treatment at the temperature of 48 ℃ for 10h to obtain graphene hydrogel fibers, and drying by supercritical carbon dioxide to obtain the graphene aerogel fibers.
Example 3:
the preparation method of the graphene aerogel fiber of the embodiment includes the following steps:
(1) preparing a pretreatment solution: heating 98% concentrated sulfuric acid by mass in an oil bath at 95 ℃, and slowly adding and dissolving potassium persulfate and phosphorus pentoxide respectively;
in the pre-oxidation treatment liquid, the concentration of potassium persulfate was 17g/mL, and the concentration of phosphorus pentoxide was 15 g/mL.
(2) Preparation of pre-oxidized graphite powder
Adding flake graphite powder into a pre-oxidation treatment liquid at 85 ℃ for reaction for 6 hours, slowly dripping water with the volume being 1.5 times that of the pre-oxidation treatment liquid into a reaction system in an ice water bath, then adding water with the volume being 12 times that of the pre-oxidation treatment liquid at one time, carrying out first water adding cooling, standing overnight, carrying out suction filtration through a microporous filter membrane, and naturally airing to obtain pre-oxidation graphite powder; wherein the concentration of the flake graphite powder in the pre-oxidation treatment liquid is 17 g/mL;
(3) preparation of graphene oxide solution
Adding pre-oxidized graphite powder into 98% concentrated sulfuric acid in mass fraction under stirring to prepare a reaction solution with the concentration of 5g/mL, wherein the mass ratio of the potassium permanganate to the pre-oxidized graphite powder is as follows: 5:1, equally dividing the potassium permanganate into 5 batches, adding the potassium permanganate into the 5 batches at an interval of 10min, controlling the temperature at 40 ℃, and stirring to react for 4 hours; adding water in an ice water bath for cooling, stirring for 5 hours, adding hydrogen peroxide until the color of the solution turns yellow, standing overnight, pouring out the supernatant, adding dilute hydrochloric acid with the mass fraction of 7%, stirring and mixing, standing, filtering and cleaning to obtain a concentrated graphene oxide solution;
(4) preparation of graphene aerogel
The graphene oxide solution is rotated at the rotating speed of 5000 r/min for 15 min; and then carrying out centrifugal separation at a rotating speed of 12000 r/min for 35min to obtain graphene oxide liquid crystal with the concentration of 20mg/mL, injecting the graphene oxide liquid crystal into a zinc nitrate coagulating bath, carrying out wet spinning to obtain a graphene oxide gel fiber aggregate, adding L-ascorbic acid with the concentration of 15% and a chitosan acetic acid solution with the concentration of 5 wt%, carrying out reduction treatment at the temperature of 55 ℃ for 15h to obtain graphene hydrogel fibers, and drying the graphene hydrogel fibers by supercritical carbon dioxide to obtain the graphene aerogel fibers.
Comparative example 1
The preparation method of the graphene aerogel fiber of the present comparative example was identical to that of example 1, except that 1 wt% of chitosan acetic acid solution was not added.
Comparative example 2
The preparation method of the graphene aerogel fiber of the comparative example is the same as that of example 1, except that the graphene oxide solution is directly injected into the zinc nitrate coagulation bath in the step (4) to perform wet spinning.
The graphene aerogel fibers prepared in examples 1 to 3 and comparative examples 1 to 2 were subjected to performance tests, and the results were as follows:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Gram weight/g/cm3 | 15.7 | 22 | 25.3 | 16.3 | 16.1 |
| Thermal conductivity/mW/(m.K) | 0.05 | 0.08 | 0.12 | 0.067 | 0.06 |
| Far infrared emissivity | 0.85 | 0.92 | 0.95 | 0.78 | 0.74 |
| Radiation heating/deg.C | 1.8 | 2.0 | 2.1 | 1.5 | 1.3 |
The graphene aerogel fiber disclosed by the invention has the advantages of low density, low thermal conductivity, high far infrared emissivity and excellent irradiation temperature rise performance, can effectively improve the heat insulation efficiency, reduces the heat loss, and has an obvious heat insulation effect.
Example 4
The graphene aerogel thermal insulation flocculus of the embodiment is mainly prepared from the following raw materials in proportion: the graphene aerogel fiber comprises flake fibers and the graphene aerogel fibers, wherein the addition amount of the graphene aerogel fibers is 3% of the mass of the flake fibers.
The preparation method of the graphene aerogel thermal insulation flocculus comprises the following steps: and uniformly mixing the flocculus fibers and the graphene aerogel fibers to prepare the graphene aerogel thermal insulation flocculus.
Example 5
The graphene aerogel thermal insulation flocculus of the embodiment is mainly prepared from the following raw materials in proportion: the graphene aerogel fiber is characterized by comprising flocculus fibers and the graphene aerogel fibers, wherein the addition amount of the graphene aerogel fibers is 5.7% of the mass of the flocculus fibers.
The preparation method of the graphene aerogel thermal insulation flocculus of the embodiment is the same as that of the embodiment 1.
Example 6
The graphene aerogel thermal insulation flocculus of the embodiment is mainly prepared from the following raw materials in proportion: the graphene aerogel fiber comprises the flocculus fiber and the graphene aerogel fiber, wherein the addition amount of the graphene aerogel fiber is 8% of the mass of the flocculus fiber.
The preparation method of the graphene aerogel thermal insulation flocculus of the embodiment is the same as that of the embodiment 1.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The preparation method of the graphene aerogel fiber is characterized by comprising the following steps:
adding the flake graphite powder into a pre-oxidation treatment solution at the temperature of 60-85 ℃ to react for 4-6 h, adding water into a reaction system for the first time in an ice water bath to cool, standing overnight, performing suction filtration, and naturally drying to obtain pre-oxidized graphite powder; wherein the concentration of the flake graphite powder in the pre-oxidation treatment liquid is 7-17 g/mL;
adding pre-oxidized graphite powder into concentrated sulfuric acid with the mass fraction of 96-98% while stirring to prepare a reaction solution with the concentration of 2-5 g/mL, adding potassium permanganate in batches, controlling the temperature at 30-40 ℃, and stirring for reaction for 1-4 hours; adding water in an ice water bath for cooling, stirring for 2-5 hours, adding hydrogen peroxide until the color of the solution turns yellow, standing overnight, pouring out the supernatant, adding dilute hydrochloric acid with the mass fraction of 3-7%, stirring and mixing, standing, filtering and cleaning to obtain a concentrated graphene oxide solution;
carrying out centrifugal separation on a graphene oxide solution to obtain graphene oxide liquid crystal with the concentration of 10-20 mg/mL, injecting the graphene oxide liquid crystal into a coagulating bath, carrying out wet spinning to obtain a graphene oxide gel fiber aggregate, adding L-ascorbic acid with the concentration of 5-15% and a chitosan acetic acid solution with the concentration of 1-5 wt%, carrying out reduction treatment at the temperature of 45-55 ℃ for 8-15 h to obtain graphene hydrogel fibers, and drying the graphene hydrogel fibers by supercritical carbon dioxide to obtain the graphene aerogel fibers.
2. The method for preparing the graphene aerogel fiber according to claim 1, wherein the preparation of the pre-oxidation treatment solution comprises: heating concentrated sulfuric acid with the mass fraction of 96-98% in an oil bath at the temperature of 80-95 ℃, and slowly adding potassium persulfate and phosphorus pentoxide respectively for dissolution;
in the pre-oxidation treatment liquid, the concentration of potassium persulfate is 5-17 g/mL, and the concentration of phosphorus pentoxide is 5-15 g/mL.
3. The method for preparing the graphene aerogel fiber according to claim 2, wherein the first water-cooling operation comprises: slowly dripping water which is 0.5-1.5 times of the volume of the preoxidation treatment solution into the reaction system, and then adding water which is 5-12 times of the volume of the preoxidation treatment solution once.
4. The method for preparing the graphene aerogel fiber according to claim 1, wherein the suction filtration is performed by using a microporous membrane.
5. The preparation method of the graphene aerogel fiber according to any one of claims 1 to 4, wherein the potassium permanganate and the pre-oxidized graphite powder are added in a mass ratio of: (2-5) 1; and equally dividing the potassium permanganate into 4-5 batches, and adding the potassium permanganate into the solution at intervals of 8-10 min in each batch.
6. The method for preparing the graphene aerogel fiber according to claim 5, wherein the graphene oxide solution is centrifuged by: rotating at 4000-5000 rpm for 5-15 min; then, the rotation speed is 10000-12000 r/min, and the time is 25-35 min.
7. A graphene aerogel fiber prepared by the method for preparing a graphene aerogel fiber according to any one of claims 1 to 6.
8. The graphene aerogel thermal insulation flocculus is characterized by being mainly prepared from the following raw materials in parts by weight: the graphene aerogel fiber of claim 7, wherein the graphene aerogel fiber is added in an amount of 3-8% by mass of the batt fiber.
9. The preparation method of the graphene aerogel thermal insulation flocculus of claim 8, comprising the following steps: and uniformly mixing the flocculus fibers and the graphene aerogel fibers to prepare the graphene aerogel thermal insulation flocculus.
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