CN113089313B - RGO/cotton sponge composite material and preparation method thereof - Google Patents

RGO/cotton sponge composite material and preparation method thereof Download PDF

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CN113089313B
CN113089313B CN202110259309.2A CN202110259309A CN113089313B CN 113089313 B CN113089313 B CN 113089313B CN 202110259309 A CN202110259309 A CN 202110259309A CN 113089313 B CN113089313 B CN 113089313B
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cotton
cotton sponge
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graphene oxide
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CN113089313A (en
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代云茜
彭晓丽
孟祥钰
孙岳明
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Southeast University
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
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Abstract

The invention discloses an RGO/cotton sponge composite material which comprises cotton sponge and reduced graphene oxide loaded on the cotton sponge, wherein the cotton sponge is composed of a plurality of layers of hierarchical structures which are stacked in sequence, a vertically extending channel is formed between every two adjacent hierarchical structures, a central channel in the cotton sponge is taken as a starting point, and the width of the channel is increased gradually towards the directions of two ends. The invention also discloses a preparation method of the RGO/cotton sponge composite material. Compared with the existing three-dimensional photothermal conversion material, the RGO/cotton sponge composite material has a three-dimensional framework structure, and has the advantages of high photothermal conversion efficiency and low heat loss by forming a structure with wide gaps at two ends and narrow gap in the middle; and the cotton fabric carrier has an effective connection structure (namely, the layers are connected through cotton fibers) and an ordered pore structure (the pore structures are vertically arranged), so that the flexible RGO/cotton sponge has excellent mechanical stability in dry and wet states, and the composite material has good mechanical stability.

Description

RGO/cotton sponge composite material and preparation method thereof
Technical Field
The invention relates to an RGO/cotton sponge composite material and a preparation method thereof.
Background
The existing three-dimensional photo-thermal conversion material (graphene-based material) has a good application prospect in the field of solar drive water evaporation application. However, the three-dimensional photothermal conversion material has the problems of large raw material consumption and high cost, and the problems of high heat loss and low photothermal conversion efficiency in the application process because the pores in the material are in a three-dimensional network structure and are arranged in a disordered manner, and the mechanical stability in a wet state is poor and the material is easily damaged in the use process because the internal structure of the material is lack of effective connection and has a disordered pore structure.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides an RGO/cotton sponge composite material and a preparation method of the RGO/cotton sponge composite material, aiming at the problems that in the prior art, a three-dimensional photothermal conversion material is high in preparation cost, high in heat loss and low in photothermal conversion efficiency due to the fact that internal through holes are arranged in a disordered mode.
The technical scheme is as follows: the RGO/cotton sponge composite material consists of cotton sponge and reduced graphene oxide loaded on the cotton sponge, wherein the cotton sponge consists of a plurality of layers of hierarchical structures which are stacked in sequence, a vertically extending channel is arranged between every two adjacent hierarchical structures, and the width of the channel increases progressively towards the directions of two ends by taking a central channel in the cotton sponge as a starting point. The reduced graphene oxide is attached to the cotton sponge through electrostatic action and hydrogen bonding, and cotton fibers are interwoven between the adjacent hierarchical structures, namely the cotton fibers transversely extending and connecting the two adjacent hierarchical structures are arranged in the channel.
Wherein the loading capacity of the reduced graphene oxide on the cotton sponge is 7-25% of the mass of the cotton sponge.
And stretching the cotton sponge by 30-70% along the stacking direction of the hierarchical structure to obtain the cotton sponge with wide channel widths at two ends and narrow channel width in the central area.
The preparation method of the RGO/cotton sponge composite material comprises the following specific steps: preparing graphene oxide, soaking a cotton sponge into a graphene oxide aqueous solution, and drying at 50-80 ℃ after soaking to obtain a cotton sponge loaded with reduced graphene oxide; then stretching the RGO/cotton sponge wetted by the ethanol at a transverse elongation of 30-70%, and finally fixing the obtained vertical channels in interval gradient arrangement by using a clamp.
Wherein the concentration of the graphene oxide aqueous solution is 1-3 mg/mL, and the soaking time is 20-50 minutes.
Wherein the drying time is 5-7 h, and the loading capacity of the reduced graphene oxide on the cotton sponge is 7% -25%.
And finally, placing the stretched RGO/cotton sponge in an oven, and drying at the temperature of not less than 75 ℃ for 3-6 h.
The mechanism of the preparation process is as follows: have many passageways along vertical extension in the cotton sponge, the width of central zone passageway is narrow in the cotton sponge, and adjacent hierarchy arranges densely promptly, and the channel width at cotton sponge both ends is wide, lies in the adjacent hierarchy of tip promptly and arranges loosely, and the dense effect in the middle of makes light pass through many times reflection in narrow clearance, improves the utilization ratio that the material was set a camera, and then increases the light-heat conversion efficiency of material, and the effect that both sides are sparse is: the two ends of the material are in contact with the outside, so that heat is easily lost, air filled in the wide space is more, the heat insulation effect of the air is good, and the heat loss of the material is reduced.
Has the advantages that: compared with the existing three-dimensional photothermal conversion material, the RGO/cotton sponge composite material has a three-dimensional framework structure, and has the advantages of high photothermal conversion efficiency and low heat loss by forming a structure with wide gaps at two ends and narrow gap in the middle; and the cotton fabric carrier has an effective connection structure (namely, the layers are connected through cotton fibers) and an ordered pore structure (the pore structures are vertically arranged), so that the flexible RGO/cotton sponge has excellent mechanical stability in dry and wet states, and the composite material has good mechanical stability.
Drawings
FIG. 1 is a diagram of a three-dimensional RGO/cotton sponge with vertically arranged channels with an RGO (reduced graphene oxide) loading of 7 wt%;
FIG. 2 is a diagram of a three-dimensional RGO/cotton sponge object with gradient-spaced vertically arranged channels and a reduced graphene oxide loading of 7 wt%;
FIG. 3 is a schematic diagram of a three-dimensional RGO/cotton sponge with gradient-spaced vertically arranged channels with a reduced graphene oxide loading of 25 wt%;
fig. 4 is a structural diagram of arrangement of the composite material vertical channels.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
Example 1
The invention discloses a method for preparing RGO/cotton sponge composite material (RGO/cotton-1), which comprises the following steps:
(1) preparing graphene oxide: placing the sodium chloride/graphite mixed powder with the sodium chloride mass fraction of 10% in an agate mortar for grinding for 10 minutes, washing with ultrapure water and performing suction filtration to remove sodium chloride solid for grinding; after the filtration is finished, placing graphite powder at 60 ℃ for drying for 24h, adding concentrated sulfuric acid with the mass fraction of 98%, preparing a graphite/concentrated sulfuric acid solution with the concentration of 12.5mg/mL, stirring for 22 hours, adding potassium permanganate into the graphite/concentrated sulfuric acid solution according to the proportion of 25% by mass fraction, and carrying out the whole process in an ice-water bath to take away a large amount of heat generated in the oxidation process; after the primary oxidation is finished, firstly stirring for 30 minutes at 40 ℃, then heating to 90 ℃, then stirring for 45 minutes, then adding ultrapure water to dilute the sulfuric acid to 35 vol%, and finally heating to 105 ℃, stirring for 25 minutes, and fully oxidizing; after the oxidation is finished, sequentially adding 28mL of ultrapure water and 2mL of hydrogen peroxide with the mass fraction of 25% into the reacted turbid liquid to remove unreacted potassium permanganate; then, using hydrochloric acid with the mass fraction of 10% to perform acid washing for 1 time, and then using ultrapure water to perform water washing for 2 times to remove the sulfuric acid which is not completely reacted; finally, transferring the colloid after water washing into a dialysis bag, dialyzing for 3 days by using ultrapure water of 18.2M omega, changing water for 3 times every day, discharging ions mixed in the synthesis process to obtain graphene oxide colloid, and placing the graphene oxide into an ultrasonic machine to perform ultrasonic treatment at 30kHz for 1 hour to disperse graphene oxide lamella;
(2) preparation of RGO/cotton sponge with three-dimensional structure: washing the layered cotton sponge with ethanol solution to remove impurities on the surface, drying at 90 deg.C for 2 hr, and cutting the sponge into cubes of 1cm × 1cm × 1 cm; then immersing the cotton sponge in an aqueous graphene oxide solution with the concentration of 1mg/mL for 20 minutes, and drying at 50 ℃ for 5 hours to obtain a cotton sponge loaded with reduced graphene oxide (7 wt%);
(3) preparation of three-dimensional RGO/cotton sponge with gradient spacing: washing the reduced graphene oxide-loaded cotton sponge with water and ethanol respectively (firstly, using water and then using ethanol) for 2-5 times, stretching the RGO/cotton sponge wetted by the ethanol at a transverse elongation of 0%, fixing the RGO/cotton sponge by using a clamp, placing the RGO/cotton sponge in an oven after fixing, and drying the RGO/cotton sponge for 3 hours at 75 ℃. The cotton sponge in the composite material does not have vertical channels arranged at gradient intervals.
Testing the evaporation performance of the driving water of the optical drive:
example 1 RGO/Cotton sponge composite was floated on a water surface contained in a flat beaker and irradiated with xenon lamp (2 kW. m)-2) The evaporation was carried out for 1 hour. During evaporation, the rate of change of water mass (v) was measured by an electronic microbalance and the evaporation calculatedHair growth efficiency (. eta.).
The results of the experiment show that the evaporation performance of the RGO/cotton sponge prepared in example 1 is shown in the following table:
Figure BDA0002969307260000031
example 2
The invention discloses a method for preparing RGO/cotton sponge composite material (RGO/cotton-2), which comprises the following steps:
(1) preparing graphene oxide: placing the sodium chloride/graphite mixed powder with the sodium chloride mass fraction of 10% in an agate mortar for grinding for 10 minutes, washing with ultrapure water and performing suction filtration to remove sodium chloride solid for grinding; after the filtration is finished, placing graphite powder at 60 ℃ for drying for 24h, adding concentrated sulfuric acid with the mass fraction of 98%, preparing a graphite/concentrated sulfuric acid solution with the concentration of 12.5mg/mL, stirring for 22 hours, adding potassium permanganate into the graphite/concentrated sulfuric acid solution according to the proportion of 25% by mass fraction, and carrying out the whole process in an ice-water bath to take away a large amount of heat generated in the oxidation process; after the primary oxidation is finished, firstly stirring for 30 minutes at 40 ℃, then heating to 90 ℃, then stirring for 45 minutes, then adding ultrapure water to dilute the sulfuric acid to 35 vol%, and finally heating to 105 ℃, stirring for 25 minutes, and fully oxidizing; after the oxidation is finished, sequentially adding 28mL of ultrapure water and 2mL of hydrogen peroxide with the mass fraction of 25% into the reacted turbid liquid to remove unreacted potassium permanganate; then, using hydrochloric acid with the mass fraction of 10% to perform acid washing for 1 time, and then using ultrapure water to perform water washing for 2 times to remove the sulfuric acid which is not completely reacted; finally, transferring the colloid after water washing into a dialysis bag, dialyzing for 3 days by using ultrapure water of 18.2M omega, changing water for 3 times every day, discharging ions mixed in the synthesis process to obtain graphene oxide colloid, and placing the graphene oxide into an ultrasonic machine to perform ultrasonic treatment at 30kHz for 1 hour to disperse graphene oxide lamella;
(2) preparation of RGO/cotton sponge with three-dimensional structure: washing the layered cotton sponge with ethanol solution to remove impurities on the surface, drying at 90 deg.C for 2 hr, and cutting the sponge into cubes of 1cm × 1cm × 1 cm; then immersing the cotton sponge in an aqueous graphene oxide solution with the concentration of 1mg/mL for 20 minutes, and drying at 50 ℃ for 5 hours to obtain a cotton sponge loaded with reduced graphene oxide (7 wt%);
(3) preparation of three-dimensional RGO/cotton sponge with gradient spacing: washing the reduced graphene oxide-loaded cotton sponge with water and ethanol for 2-5 times respectively, stretching the ethanol-wetted RGO/cotton sponge with a transverse elongation of 50% (transverse stretching in a direction perpendicular to a longitudinal channel and stretching in a direction of an arrow in FIG. 2), fixing the obtained vertical channels with gradient spacing arrangement by using a clamp, placing the RGO/cotton sponge in an oven after fixing, and drying at 75 ℃ for 3 h. The cotton sponge in the composite material is provided with vertical channels which are arranged at gradient intervals.
Testing the evaporation performance of the driving water of the optical drive:
example 2 RGO/Cotton sponge was floated on the water surface contained in a plain beaker and irradiated with xenon lamp (2 kW. m)-2) The evaporation was carried out for 1 hour. During evaporation, the rate of change of water mass (v) was measured by an electronic microbalance and the evaporation efficiency (η) was calculated.
The results of the experiment show that the evaporation performance of the RGO/cotton sponge of example 2 is shown in the following table:
Figure BDA0002969307260000041
example 3
The invention discloses a method for preparing RGO/cotton sponge composite material (RGO/cotton-3), which comprises the following steps:
(1) preparing graphene oxide: placing the sodium chloride/graphite mixed powder with the sodium chloride mass fraction of 10% in an agate mortar for grinding for 10 minutes, washing with ultrapure water and performing suction filtration to remove sodium chloride solid for grinding; after the filtration is finished, placing graphite powder at 60 ℃ for drying for 24h, adding concentrated sulfuric acid with the mass fraction of 98%, preparing a graphite/concentrated sulfuric acid solution with the concentration of 12.5mg/mL, stirring for 22 hours, adding potassium permanganate into the graphite/concentrated sulfuric acid solution according to the proportion of 25% by mass fraction, and carrying out the whole process in an ice-water bath to take away a large amount of heat generated in the oxidation process; after the primary oxidation is finished, firstly stirring for 30 minutes at 40 ℃, then heating to 90 ℃, then stirring for 45 minutes, then adding ultrapure water to dilute the sulfuric acid to 35 vol%, and finally heating to 105 ℃, stirring for 25 minutes, and fully oxidizing; after the oxidation is finished, sequentially adding 28mL of ultrapure water and 2mL of hydrogen peroxide with the mass fraction of 25% into the reacted turbid liquid to remove unreacted potassium permanganate; then, using hydrochloric acid with the mass fraction of 10% to perform acid washing for 1 time, and then using ultrapure water to perform water washing for 2 times to remove the sulfuric acid which is not completely reacted; finally, transferring the colloid after water washing into a dialysis bag, dialyzing for 3 days by using ultrapure water of 18.2M omega, changing water for 3 times every day, discharging ions mixed in the synthesis process to obtain graphene oxide colloid, and placing the graphene oxide into an ultrasonic machine to perform ultrasonic treatment at 30kHz for 1 hour to disperse graphene oxide lamella;
(2) preparation of RGO/cotton sponge with three-dimensional structure: washing the layered cotton sponge with ethanol solution to remove impurities on the surface, drying at 90 deg.C for 2 hr, and cutting the sponge into cubes of 1cm × 1cm × 1 cm; then immersing the cotton sponge in an aqueous graphene oxide solution with the concentration of 3mg/mL for 50 minutes, and drying at 80 ℃ for 7 hours to obtain a cotton sponge loaded with reduced graphene oxide (25 wt%); the loading capacity is improved by changing the concentration of the graphene oxide aqueous solution;
(3) preparation of three-dimensional RGO/cotton sponge with gradient spacing: washing the reduced graphene oxide-loaded cotton sponge with water and ethanol for 2-5 times respectively, stretching the RGO/cotton sponge wetted by the ethanol at a transverse elongation of 50% (transversely stretching along a direction perpendicular to a longitudinal channel), fixing the obtained vertical channels with gradient intervals by using a clamp, placing the RGO/cotton sponge in an oven after fixing, and drying at 75 ℃ for 4 hours. The cotton sponge in the composite material is provided with vertical channels which are arranged at gradient intervals.
Testing the evaporation performance of the driving water of the optical drive:
example 3 RGO/Cotton sponge was floated on the water surface contained in a plain beaker and irradiated with xenon lamp (2 kW. m)-2) The evaporation was carried out for 1 hour. During evaporation, the rate of change of water mass (v) was measured by an electronic microbalance and the evaporation efficiency (η) was calculated.
The results of the experiment show that the evaporation performance of the RGO/cotton sponge of example 3 is shown in the following table:
Figure BDA0002969307260000051
as can be known from experimental data of embodiments 1 to 3, the width of the channel in the central region formed by transversely stretching the cotton fabric carrier is narrow, the structure with wide channel widths at two ends can greatly improve the photothermal conversion efficiency of the composite material, and the photothermal conversion efficiency of the composite material can be further improved by improving the load capacity of the RGO on the cotton fabric carrier.

Claims (7)

1. An RGO/cotton sponge composite material, which is characterized in that: by cotton sponge and load reduction oxidation graphite alkene on cotton sponge, cotton sponge comprises the hierarchical structure that the multilayer piles up in proper order, forms vertical extension's passageway between the adjacent hierarchical structure to central passage is the starting point in the cotton sponge, and the width of passageway increases progressively in proper order to both ends direction.
2. The RGO/cotton sponge composite of claim 1, wherein: the loading capacity of the reduced graphene oxide on the cotton sponge is 7% -25% of the mass of the cotton sponge.
3. The RGO/cotton sponge composite of claim 1, wherein: the cotton sponge is stretched by 30% -70% along the stacking direction of the hierarchical structure, and the cotton sponge with wide channel widths at two ends and narrow channel width in the central area is obtained.
4. The method for preparing an RGO/cotton sponge composite material according to claim 1, which is characterized in that: preparing graphene oxide, soaking a cotton sponge into a graphene oxide aqueous solution, and drying at 50-80 ℃ after soaking to obtain a cotton sponge loaded with reduced graphene oxide; then the RGO/cotton sponge wetted by ethanol is stretched at the transverse elongation of 30-70 percent, and finally the obtained composite material is fixed by a clamp.
5. The method of preparing an RGO/cotton sponge composite as claimed in claim 4, wherein: the concentration of the graphene oxide aqueous solution is 1-3 mg/mL, and the soaking time is 20-50 minutes.
6. The method of preparing an RGO/cotton sponge composite as claimed in claim 4, wherein: the drying time is 5-7 h, and the loading capacity of the reduced graphene oxide on the cotton sponge is 7% -25%.
7. The method of preparing an RGO/cotton sponge composite as claimed in claim 4, wherein: and finally, placing the stretched RGO/cotton sponge in an oven, and drying for 3-6 h at the temperature of not less than 75 ℃.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013227694A (en) * 2012-04-25 2013-11-07 Mitsuuma:Kk Conductive three-dimensional fiber structure and method for producing the same
CN105603718A (en) * 2016-02-05 2016-05-25 济南圣泉集团股份有限公司 Composite fiber as well as preparation method and application thereof
CN106283610A (en) * 2016-08-04 2017-01-04 武汉纺织大学 A kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method
CN109183394A (en) * 2018-08-30 2019-01-11 东华大学 A kind of preparation method of photothermal conversion heat-accumulation temperature-adjustment cotton fabric

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013227694A (en) * 2012-04-25 2013-11-07 Mitsuuma:Kk Conductive three-dimensional fiber structure and method for producing the same
CN105603718A (en) * 2016-02-05 2016-05-25 济南圣泉集团股份有限公司 Composite fiber as well as preparation method and application thereof
CN106283610A (en) * 2016-08-04 2017-01-04 武汉纺织大学 A kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method
CN109183394A (en) * 2018-08-30 2019-01-11 东华大学 A kind of preparation method of photothermal conversion heat-accumulation temperature-adjustment cotton fabric
CN110093776A (en) * 2018-08-30 2019-08-06 东华大学 A kind of preparation method of photothermal conversion heat-accumulation temperature-adjustment cotton fabric

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