CN111676591A - Graphene oxide aerogel fiber fabric and preparation method and application thereof - Google Patents
Graphene oxide aerogel fiber fabric and preparation method and application thereof Download PDFInfo
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- CN111676591A CN111676591A CN202010528201.4A CN202010528201A CN111676591A CN 111676591 A CN111676591 A CN 111676591A CN 202010528201 A CN202010528201 A CN 202010528201A CN 111676591 A CN111676591 A CN 111676591A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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Abstract
A graphene oxide aerogel fiber fabric and a preparation method and application thereof belong to the technical field of nano material assembly and air filtration. The method comprises the following steps: dispersing graphene oxide into a solvent, uniformly mixing the graphene oxide and the solvent by oscillation, and performing ultrasonic treatment to obtain a graphene oxide solution; injecting the obtained graphene oxide solution into a rotary coagulating bath through a spinning head, and washing with deionized water after coagulation to obtain graphene oxide gel fibers; and (3) taking the obtained graphene oxide gel fiber, performing suction filtration to obtain a gel fiber fabric, and performing freeze drying to obtain the graphene oxide aerogel fiber fabric. The invention has the advantages of environment-friendly preparation process, room temperature operation, low energy consumption and the like, and the prepared product has nano-scale gapsThe multi-stage pore structure formed by the micron-sized pores has high filtering efficiency and PM2.5The trapping performance is good, and the method has wide application prospect in the field of air filtration.
Description
Technical Field
The invention relates to the technical field of nano material assembly and air filtration, in particular to a graphene oxide aerogel fiber fabric and a preparation method and application thereof.
Background
PM2.5The fine particles with the aerodynamic diameter less than or equal to 2.5 mu m are one of main components of the atmospheric pollutants and are also important factors influencing the air quality. It can seriously affect human health; according to the air health guidelines issued by the world health organization (WHO, 2005), prolonged exposure to PM2.5>10 μg/m3Can increase the lung cancer death rate by 95 percent. Therefore, research into effectively isolating PM2.5Meanwhile, the material with the characteristic of low pressure drop has important significance.
At present, the common filter material is that the polymer is made into fiber by an electrostatic spinning method and then is further assembled into fabric, and the obtained woven fabric material has high filtering efficiency and has excellent characteristics of antibiosis, high temperature resistance and the like. However, the pressure drop of the product prepared by the method is large during filtration, and the electrostatic spinning preparation process is complex. In addition due to PM in reality2.5The chemical composition is complex, the material is limited by the stability of the material, and the long-range use target cannot be realized. These disadvantages limit their further applications.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides the graphene oxide aerogel fiber fabric and the preparation method and application thereof, the graphene oxide aerogel fiber fabric has the advantages of environment-friendly preparation process, room-temperature operation, low energy consumption and the like, the prepared product has a hierarchical pore structure formed by nanoscale gaps and micron-sized holes, the filtering efficiency is high, and PM is formed in the surface of the product2.5The capture performance is good.
The technical scheme is as follows: a preparation method of a graphene oxide aerogel fiber fabric comprises the following steps:
dispersing graphene oxide into a solvent, oscillating and uniformly mixing for 2-15 min, and performing ultrasonic treatment for 4-30 min to obtain a graphene oxide solution with the concentration of 2-13 mg/mL;
injecting the graphene oxide solution obtained in the step one into a rotary coagulation bath with the rotating speed of 5-50 r/min through a spinning head with the diameter of 50-500 mu m at the speed of 10-1000 mu L/min, and washing with deionized water after coagulation for 1-900 s to obtain graphene oxide gel fibers;
and step three, taking the graphene oxide gel fiber obtained in the step two, performing suction filtration to obtain a gel fiber fabric, and performing freeze drying for 24-72 hours to obtain the graphene oxide aerogel fiber fabric.
Preferably, the solvent in the first step is at least one of water and ethanol.
Preferably, the coagulating bath in the second step is CaCl with the mass fraction of 1-25%2The solvent in the solution is a mixture of water and ethanol in a volume ratio of (1:9) - (9: 1).
The graphene oxide aerogel fiber fabric prepared by the method.
PM is prepared from graphene oxide aerogel fiber fabric2.5Use in a filter device.
Has the advantages that: 1. the graphene oxide gel fiber prepared by the method disclosed by the invention has nanoscale gaps, and micron-sized holes of the gel fiber fabric obtained by assembly after suction filtration form a hierarchical pore structure, so that the filtration efficiency of the graphene oxide gel fiber fabric is improved;
2. the loose and porous structure of the graphene oxide gel fiber fabric can ensure that the pressure drop is low in the filtering process, and has a good application prospect;
3. the graphene oxide used as the raw material in the method has stable chemical properties and is not easy to react with PM2.5The components react, and the fine particle pollutants can be separated from the components after being captured and simply treated, so that the effect of repeated use can be achieved;
4. the preparation method of the graphene oxide aerogel fiber fabric is environment-friendly in preparation process, low in energy consumption and capable of operating at room temperature, and the obtained graphene oxide aerogel fiber fabric is excellent in PM capture2.5The performance has wide application prospect in the field of air filtration;
5. the graphene oxide aerogel fiber fabric pair PM provided by the invention2.5The capture efficiency is 90-99%, the pressure drop is 50-210 Pa, and the prior art comprises an N95 mask, a non-woven fabric mask (for medical operation protection) and aPM pair disposable mask2.5See table below for the filtration effect of (c).
Drawings
Fig. 1 is a macroscopic photograph of a graphene oxide aerogel fiber fabric prepared in example 1 of the present invention;
fig. 2 is a scanning electron microscope image of the graphene oxide aerogel fiber fabric prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of a cross section of a single graphene oxide aerogel fiber prepared in example 1 of the present invention
Detailed Description
The invention is further described below with reference to the accompanying drawings and specific embodiments. In the embodiment of the invention, the raw material graphene oxide is prepared from crystalline flake graphite by a mature improved Hummers method.
Example 1
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 24 mg of graphene oxide into 4 mL of deionized water, uniformly mixing for 2 min by oscillation, and carrying out ultrasonic treatment for 4 min to obtain a well-dispersed graphene oxide solution with the concentration of 6 mg/mL;
(2) the graphene oxide solution obtained in step 1 was injected through a spinning nozzle with a diameter of 50 μm into a 5 r/min rotary coagulation bath (in this example, the rotary coagulation bath was 1% by mass of CaCl)2A solution, in which the solvent is a mixture of water and ethanol with a volume ratio of 1:9), solidifying for 1 s, and washing with deionized water to obtain graphene oxide gel fibers;
(3) and (3) taking the gel fiber obtained in the step (2), performing suction filtration and assembly to obtain a gel fiber fabric, and performing freeze drying for 24 hours to obtain the graphene oxide aerogel fiber fabric.
The obtained graphene oxide aerogel fiber fabric is subjected to macro-morphology and micro-morphology detection, and the results are shown in fig. 1-3. Fig. 1 is a macroscopic photograph of the prepared graphene oxide aerogel fiber fabric, which shows that the fabric has a brown appearance and a loose and porous fiber texture structure. Fig. 2 is a scanning electron microscope image of the graphene oxide aerogel fiber fabric, which shows that the inside of the fabric is assembled by a large amount of micron-sized aerogel fibers. FIG. 3 is a scanning electron microscope image of a cross section of a single graphene oxide aerogel fiber, showing the assembly of graphene oxide sheets into a flowing porous structure inside the fiber.
Performing PM capture on the prepared graphene oxide aerogel fiber fabric2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3And the PM filtration test was performed on the graphene oxide aerogel fiber fabric prepared in example 1 at a flow rate of 2.83L/min, and the obtained filtration efficiency was 96.48%, the pressure drop was 210Pa, and the filtration efficiency was maintained at 90% even after 10 cycles.
Example 2
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 24 mg of graphene oxide into a mixed solution of 3 mL of deionized water and 3 mL of ethanol, uniformly mixing for 5 min by oscillation, and performing ultrasonic treatment for 10 min to obtain a well-dispersed graphene oxide solution with the concentration of 4 mg/mL;
(2) injecting the graphene oxide solution obtained in the step (1) through a spinning head with a diameter of 100 μm at a speed of 50 μ L/min into a rotating coagulation bath with a rotating speed of 15 r/min (in the embodiment, the rotating coagulation bath is CaCl with a mass fraction of 5%)2A solution, in which the solvent is a mixture of water and ethanol with a volume ratio of 1: 3), solidifying for 50 s, and then washing with deionized water to obtain graphene oxide gel fibers;
(3) and (3) taking the gel fiber obtained in the step (2), performing suction filtration and assembly to obtain a gel fiber fabric, and performing freeze drying for 24 hours to obtain the graphene aerogel fiber fabric.
Performing PM capture on the prepared graphene oxide aerogel fiber fabric2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3And the PM filtration test was performed on the graphene oxide aerogel fiber fabric prepared in example 2 at a flow rate of 2.83L/min, and the obtained filtration efficiency was 98.24%, the pressure drop was 200 Pa, and the filtration efficiency was still maintained at 90% after 10 cycles.
Example 3
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 4 mg of graphene oxide into 2 mL of deionized water, uniformly mixing for 5 min by oscillation, and carrying out ultrasonic treatment for 10 min to obtain a well-dispersed graphene oxide solution with the concentration of 2 mg/mL;
(2) injecting the graphene oxide solution obtained in the step (1) through a spinning head with a diameter of 250 μm to a rotating coagulation bath with a rotating speed of 20 r/min at a speed of 150 μ L/min (in the embodiment, the rotating coagulation bath is CaCl with a mass fraction of 25%)2A solution, in which the solvent is a mixture of water and ethanol with a volume ratio of 9:1), solidifying for 150 s, and then washing with deionized water to obtain graphene oxide gel fibers;
(3) and (3) taking the graphene oxide gel fiber obtained in the step (2), carrying out suction filtration and assembly to obtain a gel fiber fabric, and carrying out freeze drying for 48 h to obtain the graphene aerogel fiber fabric.
Performing PM capture on the prepared graphene oxide aerogel fiber fabric2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3The graphene oxide aerogel fiber fabric prepared in example 3 was subjected to a PM filtration test at a flow rate of 2.83L/min, and the obtained filtration efficiency was 98.12%, the pressure drop was 150Pa, and the filtration efficiency was maintained at 90% even after 10 cycles.
Example 4
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 16 mg of graphene oxide into 2 mL of deionized water, uniformly mixing for 5 min by oscillation, and carrying out ultrasonic treatment for 10 min to obtain a well-dispersed graphene oxide solution with the concentration of 8 mg/mL;
(2) injecting the graphene oxide solution obtained in the step (1) through a spinning head with the diameter of 300 μm to a rotating coagulation bath with the rotating speed of 40 r/min at the speed of 300 μ L/min (in the embodiment, the rotating coagulation bath is CaCl with the mass fraction of 5%)2A solution, in which the solvent is a mixture of water and ethanol with a volume ratio of 1: 3), solidifying for 350 s, and then washing with deionized water to obtain graphene oxide gel fibers;
(3) and (3) taking the graphene oxide gel fiber obtained in the step (2), carrying out suction filtration and assembly to obtain a gel fiber fabric, and carrying out freeze drying for 48 hours to obtain the graphene oxide aerogel fiber fabric.
Performing PM capture on the prepared graphene oxide aerogel fiber fabric2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3And the PM filtration test was performed on the graphene oxide aerogel fiber fabric prepared in example 4 at a flow rate of 2.83L/min, and the obtained filtration efficiency was 97.98%, the pressure drop was 50Pa, and the filtration efficiency was maintained at 90% even after 10 cycles.
Example 5
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 20 mg of graphene oxide into 2 mL of deionized water, uniformly mixing for 12 min by oscillation, and carrying out ultrasonic treatment for 20 min to obtain a well-dispersed graphene oxide solution with the concentration of 10 mg/mL;
(2) the graphene oxide solution obtained in step (1) was injected through a spinning nozzle having a diameter of 400 μm into a 45 r/min rotary coagulation bath (in this example, the rotary coagulation bath was 5% by mass of CaCl)2A solution, in which the solvent is a mixture of water and ethanol with a volume ratio of 1: 3), solidifying for 600 s, and then washing with deionized water to obtain graphene oxide gel fibers;
(3) and (3) taking the graphene oxide gel fiber obtained in the step (2), carrying out suction filtration and assembly to obtain a gel fiber fabric, and carrying out freeze drying for 48 hours to obtain the graphene oxide aerogel fiber fabric.
Performing PM capture on the prepared graphene oxide aerogel fiber fabric2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3And the PM filtration test was performed on the graphene oxide aerogel fiber fabric prepared in example 5 at a flow rate of 2.83L/min, and the obtained filtration efficiency was 98.1%, the pressure drop was 80 Pa, and the filtration efficiency was maintained at 90% even after 10 cycles.
Example 6
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 26 mg of graphene oxide into 2 mL of deionized water, uniformly mixing for 15 min by oscillation, and carrying out ultrasonic treatment for 30 min to obtain a well-dispersed graphene oxide solution with the concentration of 13 mg/mL;
(2) injecting the graphene oxide solution obtained in the step (1) into a rotary coagulation bath with the speed of 1000 muL/min and the diameter of 500 muM through a spinning head with the diameter of 50 r/min (in the embodiment, the rotary coagulation bath is CaCl with the mass fraction of 5%)2A solution, in which the solvent is a mixture of water and ethanol with a volume ratio of 1: 3), solidifying for 900 s, and then washing with deionized water to obtain graphene oxide gel fibers;
(3) and (3) taking the graphene oxide gel fiber obtained in the step (2), carrying out suction filtration and assembly to obtain a gel fiber fabric, and carrying out freeze drying for 72 h to obtain the graphene aerogel fiber fabric.
The graphene oxide aerogel fiber fabric prepared by the method and an N95 mask in the prior art (meeting the national GB/T23465-2009 practical performance evaluation of respiratory protection products [ S ]]Mask required by test), disposable mask, non-woven mask (hospital operation protection) for capturing PM2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3The graphene oxide aerogel fiber fabric prepared in example 6 and an N95 mask (satisfying national GB/T23465-2009, evaluation of practical performance of respiratory protection product [ S ] were applied at a flow rate of 2.83L/min]Mask required for testing), disposable mask, non-woven fabric mask (hospital operation protection) were subjected to PM filtration test, with the following results: the graphene oxide aerogel fiber fabric prepared by the embodiment has the filtering efficiency of 99.34% and the pressure drop of 210Pa, and can be recycled for 10 times and still maintain the filtering efficiency of 90%. N95 mask (satisfying national GB/T23465-2009. evaluation of practical performance of respiratory protection article [ S ]]Mask required for testing) filtration efficiency was 94.9% and pressure drop was 510 Pa. The disposable mask efficiency was 32.9% and the pressure drop was 290 Pa. The efficiency of the non-woven fabric mask (medical operation protection) is 96.9 percent, and the pressure drop is 645 Pa.
Comparative example 1
The preparation method of the graphene oxide aerogel fiber fabric in the embodiment comprises the following steps:
(1) dispersing 26 mg of graphene oxide into 2 mL of deionized water, uniformly mixing for 15 min by oscillation, and carrying out ultrasonic treatment for 30 min to obtain a well-dispersed graphene oxide solution with the concentration of 13 mg/mL;
(2) injecting the graphene oxide solution obtained in the step (1) into a rotary coagulation bath (in the embodiment, the rotary coagulation bath is a CaCl2 solution with the mass fraction of 5%, and the solvent in the solution is a mixture of water and ethanol with the volume ratio of 1: 3) with the speed of 1000 [ mu ] L/min and the diameter of 500 [ mu ] m through a spinning head, and washing with deionized water after 20 min of coagulation to obtain graphene oxide gel fibers;
(3) and (3) taking the graphene oxide gel fiber obtained in the step (2), carrying out suction filtration and assembly to obtain a gel fiber fabric, and carrying out freeze drying for 72 h to obtain the graphene aerogel fiber fabric.
Performing PM capture on the prepared graphene oxide aerogel fiber fabric2.5And (4) detecting the performance, wherein the result is as follows:
using cigarette as PM generating source2.5The concentration is 500-3000 mu g/m3And PM treatment is carried out on the graphene oxide aerogel fiber fabric prepared in the comparative example under the condition that the flow rate is 2.83L/minAnd (4) a filtration test shows that the filtration efficiency of the obtained graphene oxide aerogel fiber fabric is 86.1%, and the pressure drop is 105 Pa. Due to the fact that the solidification time is too long, the graphene fibers are too tightly solidified, the formed micron-sized aperture is too small, and the method is not suitable for PM2.5And (4) capturing.
In conclusion, the graphene oxide aerogel fiber fabric prepared by the invention has a hierarchical pore structure, the pore size is tens of micrometers, and the fiber diameter is hundreds of micrometers. The pore size can be adjusted by the concentration of the graphene oxide solution and the solidification time, and generally, the larger the concentration of the graphene oxide solution and the longer the solidification time, the smaller the pore size obtained. The diameter of the fiber can be adjusted by the diameter of the spinneret, the advancing speed of the injection pump, and the rotating speed of the coagulation bath, and generally, the larger the diameter of the spinneret, the faster the advancing speed of the injection pump, and the slower the rotating speed of the coagulation bath, the larger the diameter of the fiber.
The above are preferred embodiments of the present invention, and all changes made according to the technical scheme of the present invention that produce functional effects do not exceed the scope of the technical scheme of the present invention belong to the protection scope of the present invention.
Claims (5)
1. The preparation method of the graphene oxide aerogel fiber fabric is characterized by comprising the following steps:
dispersing graphene oxide into a solvent, oscillating and uniformly mixing for 2-15 min, and performing ultrasonic treatment for 4-30 min to obtain a graphene oxide solution with the concentration of 2-13 mg/mL;
injecting the graphene oxide solution obtained in the step one into a rotary coagulation bath with the rotating speed of 5-50 r/min through a spinning head with the diameter of 50-500 mu m at the speed of 10-1000 mu L/min, and washing with deionized water after coagulation for 1-900 s to obtain graphene oxide gel fibers;
and step three, taking the graphene oxide gel fiber obtained in the step two, performing suction filtration to obtain a gel fiber fabric, and performing freeze drying for 24-72 hours to obtain the graphene oxide aerogel fiber fabric.
2. The method for preparing a graphene oxide aerogel fiber fabric according to claim 1, wherein the solvent in the first step is at least one of water and ethanol.
3. The preparation method of the graphene oxide aerogel fiber fabric, according to claim 1, wherein the coagulation bath in the second step is 1-25% by mass of CaCl2The solvent in the solution is a mixture of water and ethanol in a volume ratio of (1:9) - (9: 1).
4. A graphene oxide aerogel fiber fabric prepared based on the method of any of claims 1-3.
5. Preparation of PM from the graphene oxide aerogel fiber fabric as claimed in claim 42.5Use in a filter device.
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| WO2023108378A1 (en) * | 2021-12-14 | 2023-06-22 | 浙江大学 | Aerogel fiber having specific section morphology feature, and preparation method and device therefor |
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Application publication date: 20200918 |