CN120586830B - Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption - Google Patents

Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption

Info

Publication number
CN120586830B
CN120586830B CN202511090789.9A CN202511090789A CN120586830B CN 120586830 B CN120586830 B CN 120586830B CN 202511090789 A CN202511090789 A CN 202511090789A CN 120586830 B CN120586830 B CN 120586830B
Authority
CN
China
Prior art keywords
modified
powder
textile
oil
shell powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202511090789.9A
Other languages
Chinese (zh)
Other versions
CN120586830A (en
Inventor
周蓉
周衡书
刘超
陈曦
李东衡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Institute of Engineering
Original Assignee
Hunan Institute of Engineering
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hunan Institute of Engineering filed Critical Hunan Institute of Engineering
Priority to CN202511090789.9A priority Critical patent/CN120586830B/en
Publication of CN120586830A publication Critical patent/CN120586830A/en
Application granted granted Critical
Publication of CN120586830B publication Critical patent/CN120586830B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • D04H1/4282—Addition polymers
    • D04H1/43—Acrylonitrile series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28028—Particles immobilised within fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • 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
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/32—Hydrocarbons, e.g. oil
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00—Water conservation; Efficient water supply; Efficient water use
    • Y02A20/20—Controlling water pollution; Waste water treatment
    • Y02A20/204—Keeping clear the surface of open water from oil spills

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Textile Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Thermal Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

本发明公开了吸油材料领域的一种纺织基吸油材料及其在重油光热吸收中的应用，材料制备方法为：取多壁碳纳米管与改性Fe3O4粉末，加入十二烷基苯磺酸钠水溶液处理得悬浮液；取聚丙烯腈纤维加入至N，N‑二甲基甲酰胺中，再加入悬浮液，并滴加疏水改性剂和催化剂，得静电纺丝液，纺丝成网，再取改性千足虫壳粉喷洒至纤维网表面并固化；取纤维网经高温处理即得纺织基吸油材料。该吸油材料采用多壁碳纳米管和改性Fe3O4粉末双重光热协同因子，使材料整体光热效率大幅增强，从而解决常规吸油材料针对重油的吸油效率较低的问题，另外采用多孔纺织基结构，且表面经疏水改性处理，能够表现出优良的疏水亲油性，有助于实现高效的油水分离。

The invention discloses a kind of textile-based oil-absorbing material in the field of oil-absorbing material and its application in heavy oil photothermal absorption, and the material preparation method is as follows: take multi-walled carbon nanotubes and modified Fe 3 O 4 powder, add sodium dodecylbenzene sulfonate aqueous solution to process to obtain suspension; take polyacrylonitrile fiber and add it to N, N-dimethylformamide, then add suspension, and drip hydrophobic modifier and catalyst to obtain electrostatic spinning solution, spin into web, then take modified millipede shell powder and spray it on the fiber web surface and solidify; take fiber web and obtain textile-based oil-absorbing material through high temperature treatment. The oil-absorbing material adopts multi-walled carbon nanotubes and modified Fe 3 O 4 powder dual photothermal synergistic factors, so that the overall photothermal efficiency of the material is greatly enhanced, thereby solving the problem that conventional oil-absorbing materials have low oil absorption efficiency for heavy oil, and adopts porous textile-based structure in addition, and the surface is hydrophobically modified, can show excellent hydrophobic lipophilicity, and helps to achieve efficient oil-water separation.

Description

Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption
Technical Field
The invention relates to the field of oil absorption materials, in particular to a textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption.
Background
In order to protect the ecosystem, there is an urgent need to develop an efficient and environmentally friendly oil recovery process. Unfortunately, traditional petroleum leak recovery methods, such as mechanical techniques, chemical dispersion and bioremediation, not only have low separation efficiency, but may also cause secondary pollution to the environment. Physical adsorption is considered a good alternative to oil removal because it is effective in recovering oil from water. Various porous oil absorbing materials have been proposed for oil stain cleaning, such as modified commercial sponges, modified foams, aerogels, biomass materials, and the like. The quick oil stain absorption can effectively save the oil stain cleaning time and reduce the oil stain diffusion range, thereby reducing the environmental damage caused by the oil stains and saving the cost as much as possible.
However, the porous absorbent materials described above generally exhibit a high absorption capacity for oils of low viscosity (typically less than 1000 mPa-s), but are not suitable for the high viscosity leakage of oil (103-105 mPa s at room temperature) at about 40% in reality. High viscosity oils, such as heavy oils, are difficult to effectively diffuse and penetrate into the internal pores of porous absorbent materials, resulting in a significant reduction in oil absorption rate. At the same time, too high a viscosity may also destroy the internal pore structure of the absorbent material, reducing its efficiency of use. Therefore, the development of the absorbing material suitable for high-viscosity oil spill treatment has important practical significance and scientific value.
It is well known that the viscosity of heavy oils generally decreases as the oil temperature increases, while photothermal material systems are capable of directly converting sustainable solar energy into thermal energy, which can reduce the viscosity of heavy oils, thereby promoting heavy oil flow and increasing heavy oil extraction efficiency. The currently available photothermal conversion may be achieved by using carbon-based materials, such as graphene oxide, carbon nanotubes, etc. Based on the technical direction, the light-heat conversion material is applied to the oil absorption material, so that the heavy oil absorption effect can be improved theoretically. However, there is currently little research in this regard and similar oil absorbing materials are lacking in the marketplace.
Disclosure of Invention
The invention aims to provide a textile-based oil absorption material and application thereof in photo-thermal absorption of heavy oil, and solves the problem that the conventional oil absorption material has low oil absorption efficiency for heavy oil.
The invention realizes the above purpose through the following technical scheme:
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multiwall carbon nanotube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under an ice bath condition to form a homogeneous suspension;
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment to obtain an electrostatic spinning solution;
S3, carrying out electrostatic spinning and net forming by using the electrostatic spinning solution to obtain a fiber net, uniformly spraying modified euphorbia shell powder accounting for 4-8% of the fiber net to the surface of the fiber net, heating the fiber net to 110-120 ℃ and maintaining for 6-8S, so that the fiber net is softened and combined with the modified euphorbia shell powder;
S4, placing the fiber net in an air atmosphere at 270-280 ℃ for pre-oxidation for 1.5-2.5 hours, placing the fiber net in a high-temperature tube furnace, heating to 750-800 ℃ at a heating rate of 3-5 ℃ per minute under the protection of inert gas, preserving heat for 1-2 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorbing material.
The further improvement is that in the step S1, the mass ratio of the multi-wall carbon nano tube to the modified Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 1-3:0.5-1.5:50, and the sodium dodecyl benzene sulfonate accounts for 0.3-0.5% of the total mass of the multi-wall carbon nano tube and the modified Fe 3O4 powder.
The further improvement is that in the step S1, the preparation method of the modified Fe 3O4 powder comprises the following steps:
adding polyoxyethylene nonylphenol ether accounting for 0.04-0.08% of the volume of cyclohexane into cyclohexane, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of ferric chloride hexahydrate accounting for 3-5% of the volume of cyclohexane and having the concentration of 0.4-0.8mol/L and ammonia accounting for 6-8% of the volume of cyclohexane and having the concentration of 1.5-2.5mol/L into the emulsion, and stirring and reacting to obtain Fe 3O4 particle dispersion;
Dripping ethyl orthosilicate accounting for 16-20% of the volume of cyclohexane and ammonia water accounting for 15-20% of the volume of cyclohexane and having the concentration of 1.5-2.5mol/L into the Fe 3O4 particle dispersion liquid, and stirring and reacting to obtain Fe 3O4 composite particles with the surfaces coated with silicon dioxide;
Separating Fe 3O4 composite particles, adding the composite particles into ethanol according to the proportion of 1g of the particles to 50-60mL of ethanol, heating to 55-60 ℃ and uniformly stirring, adding hexamethyldisilazane accounting for 12-16% of the volume of the ethanol, heating to 120-130 ℃ and stirring for reacting for 1.5-2.5h;
And separating and taking Fe 3O4 composite particles, and cleaning and drying to obtain modified Fe 3O4 powder.
The further improvement is that in the step S1, the ultrasonic treatment has the frequency of 35-40kHz, the power of 500-600W and the treatment time of 2-3h.
The further improvement is that in the step S2, the mass ratio of the polyacrylonitrile fiber, the N, N-dimethylformamide, the suspension, the polydimethylsiloxane hydrophobic modifier and the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 10-12:90-100:2-3:0.8-0.9:0.01-0.015.
The further improvement is that in the step S2, the pressure of the vacuum defoaming treatment is-0.1 MPa, and the time is 2-3h.
The further improvement is that in the step S3, the voltage of the electrostatic spinning is 15-25kV, the liquid supply speed is 2-4mL/h, the receiving distance is 12-18cm, the inner diameter of the needle head is 0.3-0.5mm, and the rotating speed of the dynamic receiving aluminum roller is 10-50rpm.
The preparation method of the modified Qianchu insect shell powder is characterized by further improving in step S3, wherein the preparation method comprises the steps of cleaning artificially cultured Qianchu insect, removing impurities, soaking in 0.5-1.5M HCl solution for 0.5-1.5h, taking out, freeze-drying and crushing to obtain shell powder, taking out the shell powder, soaking in ethanol solution containing 8-12wt% of tetraethoxysilane for 1.5-2h, taking out the shell powder, solidifying at 50-60 ℃ for 8-12h, soaking in acetic acid solution containing 1.5-2wt% of chitosan and 0.8-1.2wt% of boric acid, stirring for reacting at 50-60 ℃ for 2-4h, finally taking out the shell powder, washing and drying to obtain the modified Qianchu insect shell powder.
The further improvement is that the particle size of the shell powder is 60-80 mu m.
The invention also provides application of the textile-based oil absorption material in heavy oil photo-thermal absorption.
The invention has the beneficial effects that:
(1) The oil absorption material adopts double photo-thermal synergistic factors of the multi-wall carbon nano tube and the modified Fe 3O4 powder, and the wide spectrum absorption characteristic of the multi-wall carbon nano tube and the near infrared response characteristic of the modified Fe 3O4 powder are utilized, so that the overall photo-thermal efficiency of the material is greatly enhanced, and the problem that the oil absorption efficiency of the conventional oil absorption material for heavy oil is lower is effectively solved.
The modified Fe 3O4 powder is coated by a silica thin layer and subjected to surface treatment by hexamethyldisilazane, so that the dispersibility and the compatibility of the powder are greatly improved on the basis of not affecting the near infrared response characteristic, the compounding effect of the powder and the multiwall carbon nano tube is ensured, and sedimentation and agglomeration are avoided.
(2) The oil absorption material adopts a porous textile base structure, and the surface of the oil absorption material is subjected to hydrophobic modification treatment, so that the oil absorption material can show excellent hydrophobic and oleophilic properties, and is favorable for realizing efficient oil-water separation.
Specifically, the modified Qianchu insect hull powder is loaded on the surface of the fiber net, the porous framework is further perfected after carbonization, the hydrophobic oil absorption performance of the material is enhanced, and the self-modification treatment of the modified Qianchu insect hull powder can reduce ash (CaO) after carbonization, improve toughness, ensure that the modified Qianchu insect hull powder can be stably loaded on the surface of the fiber net, and further ensure that the hydrophobic oil absorption effect is exerted.
Drawings
FIG. 1 is a transmission electron microscope image of a modified Fe 3O4 powder;
FIG. 2 is a digital representation of the various groups of textile-based oil absorbing materials as they contact a surface of a water drop;
figure 3 is a digital representation of the various groups of textile-based oil absorbing materials as they contact the surface of the oil droplets.
Detailed Description
The present application will be described in further detail with reference to the accompanying drawings, wherein it is to be understood that the following detailed description is for the purpose of further illustrating the application only and is not to be construed as limiting the scope of the application, as various insubstantial modifications and adaptations of the application to those skilled in the art can be made in light of the foregoing disclosure.
1. Main materials
Multiwall carbon nanotubes purchased from Shanghai detection field New Material technologies Co., ltd;
ferric chloride hexahydrate, feCl 3·6H2 O, available from Wuhan Xingzhong Chengcheng technology Co., ltd;
Sodium dodecyl benzene sulfonate, available from Jinan Xin chemical Co., ltd;
polyacrylonitrile fiber with a diameter of about 12 μm is purchased from super engineering materials Co., ltd;
N, N-dimethylformamide available from Shandong Magnomonic chemical Co., ltd;
Polydimethylsiloxane having a molecular weight of 15000, available from King chemical Co., ltd. In Guangzhou;
dibutyl tin dilaurate available from Shandong Yao homohousing Co., ltd;
and the Qianchou insect is purchased from a market shop of Huperzia serrata agricultural and sideline products in the city of Bozhou.
2. Experiment was conducted
Example 1
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multi-wall carbon nano tube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under ice bath conditions (the frequency is 35kHz, the power is 500W, the treatment time is 3 h) to form a homogeneous suspension, wherein the mass ratio of the multi-wall carbon nano tube, the modified Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 1:0.5:50, and the sodium dodecyl benzene sulfonate in the sodium dodecyl benzene sulfonate aqueous solution accounts for 0.3% of the total mass of the multi-wall carbon nano tube and the modified Fe 3O4 powder;
The preparation method of the modified Fe 3O4 powder comprises the steps of taking cyclohexane, adding nonylphenol polyoxyethylene ether accounting for 0.04% of the cyclohexane volume, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of hexahydrate with concentration of 0.8mol/L accounting for 3% of the cyclohexane volume and aqueous ammonia with concentration of 2.5mol/L accounting for 6% of the cyclohexane volume into the emulsion, stirring and reacting to obtain Fe 3O4 particle dispersion, dropwise adding tetraethoxysilane accounting for 16% of the cyclohexane volume and aqueous ammonia with concentration of 2.5mol/L accounting for 15% of the cyclohexane volume into the Fe 3O4 particle dispersion, stirring and reacting to obtain Fe 3O4 composite particles with surface coated silicon dioxide, separating and taking Fe 3O4 composite particles, adding 1g of particles into 50mL of ethanol, heating to 55 ℃ and stirring uniformly, adding hexamethyldisilazane accounting for 12% of the ethanol volume, heating to 120 ℃ and stirring and reacting for 2.5 hours, separating and taking Fe 3O4 composite particles, and washing and drying to obtain the modified Fe 3O4 powder;
s2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment (the pressure is-0.1 MPa and the time is 2 h) to obtain an electrostatic spinning solution, wherein the mass ratio of the polyacrylonitrile fibers to the N, N-dimethylformamide to the suspension to the polydimethylsiloxane hydrophobic modifier to the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 10:90:2:0.8:0.01;
S3, carrying out electrostatic spinning and net forming by using the electrostatic spinning solution, wherein the electrostatic spinning voltage is 15kV, the liquid supply speed is 2mL/h, the receiving distance is 12cm, the inner diameter of a needle head is 0.3mm, the rotating speed of a dynamic receiving aluminum roller is 10rpm, a fiber net is obtained, then modified euphorbia shell powder accounting for 4% of the fiber net mass is uniformly sprayed on the surface of the fiber net, the fiber net is heated to 110 ℃ and maintained for 8 seconds, and the fiber net is softened and combined with the modified euphorbia shell powder;
The preparation method of the modified Qianchu insect shell powder comprises the steps of cleaning artificially cultured Qianchu insect, removing impurities, soaking in 0.3M HCl solution for 1.5h, taking out, freeze-drying and crushing to obtain shell powder with the particle size of about 60 mu M, taking out the shell powder, soaking the shell powder in ethanol solution containing 8wt% of ethyl orthosilicate for 2h, taking out the shell powder, solidifying the shell powder at 50 ℃ for 12h, soaking the shell powder in acetic acid solution containing 1.5wt% of chitosan and 0.8wt% of boric acid, stirring and reacting for 4h at 50 ℃, finally taking out the shell powder, washing and drying to obtain the modified Qianchu insect shell powder;
s4, placing the fiber net in an air atmosphere at 270 ℃ for pre-oxidation for 2.5 hours, placing the fiber net in a high-temperature tube furnace, heating to 750 ℃ at a heating rate of 3 ℃ per minute under the protection of inert gas, preserving heat for 2 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorption material.
Example 2
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multi-wall carbon nano tube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under ice bath conditions (the frequency is 38kHz, the power is 550W, the treatment time is 2.5 h) to form a homogeneous suspension, wherein the mass ratio of the multi-wall carbon nano tube, the modified Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 2:1:50, and the sodium dodecyl benzene sulfonate in the sodium dodecyl benzene sulfonate aqueous solution accounts for 0.4% of the total mass of the multi-wall carbon nano tube and the modified Fe 3O4 powder;
The preparation method of the modified Fe 3O4 powder comprises the steps of taking cyclohexane, adding nonylphenol polyoxyethylene ether accounting for 0.06% of the cyclohexane volume, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of hexamethyldisilazane accounting for 4% of the cyclohexane volume and the concentration of 0.6mol/L into the emulsion, stirring and reacting to obtain Fe 3O4 particle dispersion, dropwise adding tetraethoxysilane accounting for 18% of the cyclohexane volume and ammonia water accounting for 2mol/L of the cyclohexane volume into the Fe 3O4 particle dispersion, stirring and reacting to obtain Fe 3O4 composite particles with surface coated silicon dioxide, separating and taking Fe 3O4 composite particles, adding 1g of particles into ethanol according to the proportion of 55mL of ethanol, heating to 58 ℃ and stirring uniformly, then adding hexamethyldisilazane accounting for 14% of the ethanol volume, heating to 125 ℃ and stirring and reacting for 2h, separating and taking 3O4 composite particles, washing and drying to obtain modified Fe 3O4 powder, and obtaining spherical powder with a transmission electron microscope (JEM 1200- 3O4) which has obvious characteristics, wherein the appearance is shown by the graph, and the appearance of the spherical powder is not shown by the graph, and the appearance of the spherical powder is obtained.
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment (the pressure is-0.1 MPa and the time is 2.5 h) to obtain an electrostatic spinning solution, wherein the mass ratio of the polyacrylonitrile fibers to the N, N-dimethylformamide to the suspension to the polydimethylsiloxane hydrophobic modifier to the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 11:95:2.5:0.8:0.012;
s3, carrying out electrostatic spinning and net forming by using the electrostatic spinning solution, wherein the electrostatic spinning voltage is 20kV, the liquid supply speed is 3mL/h, the receiving distance is 15cm, the inner diameter of a needle head is 0.4mm, the rotating speed of a dynamic receiving aluminum roller is 30rpm, a fiber net is obtained, then modified euphorbia shell powder accounting for 6% of the fiber net mass is uniformly sprayed on the surface of the fiber net, the fiber net is heated to 115 ℃ and maintained for 7S, and the fiber net is softened and combined with the modified euphorbia shell powder;
The preparation method of the modified Qianchu insect shell powder comprises the steps of cleaning artificially cultured Qianchu insect, removing impurities, soaking in 0.4M HCl solution for 1h, taking out, freeze-drying and crushing to obtain shell powder with the particle size of about 70 mu M, taking out the shell powder, soaking the shell powder in ethanol solution containing 10wt% of tetraethoxysilane for 1.8h, taking out the shell powder, solidifying the shell powder at 55 ℃ for 10h, soaking the shell powder in acetic acid solution containing 1.8wt% of chitosan and 1wt% of boric acid, stirring at 55 ℃ for 3h, taking out the shell powder, washing with water, and drying to obtain modified Qianchu insect shell powder;
S4, placing the fiber net in an air atmosphere at 275 ℃ for pre-oxidation for 2 hours, placing the fiber net in a high-temperature tube furnace, heating to 780 ℃ at a heating rate of 4 ℃ per minute under the protection of inert gas, preserving heat for 1.5 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorption material.
Example 3
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multi-wall carbon nano tube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under ice bath conditions (the frequency is 40kHz, the power is 600W, the treatment time is 2 h) to form a homogeneous suspension, wherein the mass ratio of the multi-wall carbon nano tube, the modified Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 3:1.5:50, and the sodium dodecyl benzene sulfonate in the sodium dodecyl benzene sulfonate aqueous solution accounts for 0.5% of the total mass of the multi-wall carbon nano tube and the modified Fe 3O4 powder;
The preparation method of the modified Fe 3O4 powder comprises the steps of taking cyclohexane, adding polyoxyethylene nonylphenol ether accounting for 0.08% of the cyclohexane volume, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of ferric chloride hexahydrate accounting for 5% of the cyclohexane volume and the concentration of 0.4mol/L and ammonia water accounting for 8% of the cyclohexane volume and the concentration of 1.5mol/L into the emulsion, stirring and reacting to obtain Fe 3O4 particle dispersion, dropwise adding ethyl orthosilicate accounting for 20% of the cyclohexane volume and ammonia water accounting for 1.5mol/L of the cyclohexane volume into the Fe 3O4 particle dispersion, stirring and reacting to obtain Fe 3O4 composite particles with silicon dioxide coated on the surface, separating and taking Fe 3O4 composite particles, adding the Fe 3O4 composite particles into ethanol according to the proportion of 1g of 60mL of ethanol, heating to 60 ℃, stirring uniformly, adding hexamethyldisilazane accounting for 16% of the ethanol volume, heating to 130 ℃, stirring and reacting for 1.5h, separating and taking Fe 3O4 composite particles, washing and drying to obtain the modified Fe 3O4 powder;
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment (the pressure is-0.1 MPa and the time is 3 h) to obtain an electrostatic spinning solution, wherein the mass ratio of the polyacrylonitrile fibers to the N, N-dimethylformamide to the suspension to the polydimethylsiloxane hydrophobic modifier to the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 12:100:2:0.9:0.015;
S3, carrying out electrostatic spinning and net forming by using the electrostatic spinning solution, wherein the electrostatic spinning voltage is 25kV, the liquid supply speed is 4mL/h, the receiving distance is 18cm, the inner diameter of a needle head is 0.5mm, the rotating speed of a dynamic receiving aluminum roller is 50rpm, a fiber net is obtained, then modified euphorbia shell powder accounting for 8% of the fiber net mass is uniformly sprayed on the surface of the fiber net, the fiber net is heated to 120 ℃ and maintained for 6S, and the fiber net is softened and combined with the modified euphorbia shell powder;
The preparation method of the modified Qianchu insect shell powder comprises the steps of cleaning artificially cultured Qianchu insect, removing impurities, soaking in 0.5M HCl solution for 0.5h, taking out, freeze-drying and crushing to obtain shell powder with the particle size of about 80 mu M, taking out the shell powder, immersing the shell powder in ethanol solution containing 12wt% of ethyl orthosilicate for 1.5h, taking out the shell powder, solidifying at 60 ℃ for 8h, immersing the shell powder in acetic acid solution containing 2wt% of chitosan and 1.2wt% of boric acid, stirring at 60 ℃ for 2h, finally taking out the shell powder, washing with water, and drying to obtain modified Qianchu insect shell powder;
s4, placing the fiber net in an air atmosphere at 280 ℃ for pre-oxidation for 1.5 hours, placing the fiber net in a high-temperature tube furnace, heating to 800 ℃ at a temperature rising rate of 5 ℃ per minute under the protection of inert gas, preserving heat for 1 hour, and finally naturally cooling to room temperature to obtain the textile-based oil absorption material.
Comparative example 1
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multi-wall carbon nano tube with Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under an ice bath condition (the frequency is 38kHz, the power is 550W, the treatment time is 2.5 h) to form a homogeneous suspension, wherein the mass ratio of the multi-wall carbon nano tube to the Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 2:1:50, and the sodium dodecyl benzene sulfonate in the sodium dodecyl benzene sulfonate aqueous solution accounts for 0.4% of the total mass of the multi-wall carbon nano tube and the Fe 3O4 powder;
The preparation method of the Fe 3O4 powder comprises the steps of taking cyclohexane, adding polyoxyethylene nonylphenol ether accounting for 0.06% of the volume of the cyclohexane, stirring and dispersing uniformly to obtain emulsion, then dripping an aqueous solution of ferric chloride hexahydrate accounting for 4% of the volume of the cyclohexane and having the concentration of 0.6mol/L and ammonia water accounting for 7% of the volume of the cyclohexane and having the concentration of 2mol/L into the emulsion, stirring and reacting to obtain Fe 3O4 particle dispersion liquid, separating Fe 3O4 particles, cleaning and drying to obtain Fe 3O4 powder;
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment (the pressure is-0.1 MPa and the time is 2.5 h) to obtain an electrostatic spinning solution, wherein the mass ratio of the polyacrylonitrile fibers to the N, N-dimethylformamide to the suspension to the polydimethylsiloxane hydrophobic modifier to the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 11:95:2.5:0.8:0.012;
s3, carrying out electrostatic spinning and net forming by using the electrostatic spinning solution, wherein the electrostatic spinning voltage is 20kV, the liquid supply speed is 3mL/h, the receiving distance is 15cm, the inner diameter of a needle head is 0.4mm, the rotating speed of a dynamic receiving aluminum roller is 30rpm, a fiber net is obtained, then modified euphorbia shell powder accounting for 6% of the fiber net mass is uniformly sprayed on the surface of the fiber net, the fiber net is heated to 115 ℃ and maintained for 7S, and the fiber net is softened and combined with the modified euphorbia shell powder;
The preparation method of the modified Qianchu insect shell powder comprises the steps of cleaning artificially cultured Qianchu insect, removing impurities, soaking in 0.4M HCl solution for 1h, taking out, freeze-drying and crushing to obtain shell powder with the particle size of about 70 mu M, taking out the shell powder, soaking the shell powder in ethanol solution containing 10wt% of tetraethoxysilane for 1.8h, taking out the shell powder, solidifying the shell powder at 55 ℃ for 10h, soaking the shell powder in acetic acid solution containing 1.8wt% of chitosan and 1wt% of boric acid, stirring at 55 ℃ for 3h, taking out the shell powder, washing with water, and drying to obtain modified Qianchu insect shell powder;
S4, placing the fiber net in an air atmosphere at 275 ℃ for pre-oxidation for 2 hours, placing the fiber net in a high-temperature tube furnace, heating to 780 ℃ at a heating rate of 4 ℃ per minute under the protection of inert gas, preserving heat for 1.5 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorption material.
Comparative example 2
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multi-wall carbon nano tube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under ice bath conditions (the frequency is 38kHz, the power is 550W, the treatment time is 2.5 h) to form a homogeneous suspension, wherein the mass ratio of the multi-wall carbon nano tube, the modified Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 2:1:50, and the sodium dodecyl benzene sulfonate in the sodium dodecyl benzene sulfonate aqueous solution accounts for 0.4% of the total mass of the multi-wall carbon nano tube and the modified Fe 3O4 powder;
The preparation method of the modified Fe 3O4 powder comprises the steps of taking cyclohexane, adding polyoxyethylene nonylphenol ether accounting for 0.06% of the volume of the cyclohexane, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of ferric chloride hexahydrate accounting for 4% of the volume of the cyclohexane and having the concentration of 0.6mol/L and aqueous ammonia accounting for 7% of the volume of the cyclohexane and having the concentration of 2mol/L into the emulsion, stirring and reacting to obtain Fe 3O4 particle dispersion liquid, dropwise adding tetraethoxysilane accounting for 18% of the volume of the cyclohexane and aqueous ammonia accounting for 18% of the volume of the cyclohexane and having the concentration of 2mol/L into the Fe 3O4 particle dispersion liquid, stirring and reacting to obtain Fe 3O4 composite particles with silicon dioxide coated on the surface, separating and taking Fe 3O4 composite particles, adding 1g of particles into ethanol at the proportion of 55mL of ethanol, heating to 58 ℃ and stirring uniformly, adding hexamethyldisilazane accounting for 14% of the volume of the ethanol, heating to 125 ℃ and stirring and reacting for 2h, separating and taking Fe 3O4 composite particles, and washing and drying to obtain modified Fe 3O4 powder;
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment (the pressure is-0.1 MPa and the time is 2.5 h) to obtain an electrostatic spinning solution, wherein the mass ratio of the polyacrylonitrile fibers to the N, N-dimethylformamide to the suspension to the polydimethylsiloxane hydrophobic modifier to the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 11:95:2.5:0.8:0.012;
s3, carrying out electrostatic spinning and reticulation by using the electrostatic spinning solution, wherein the voltage of electrostatic spinning is 20kV, the liquid supply speed is 3mL/h, the receiving distance is 15cm, the inner diameter of a needle is 0.4mm, and the rotating speed of a dynamic receiving aluminum roller is 30rpm, so that a fiber web is obtained;
S4, placing the fiber net in an air atmosphere at 275 ℃ for pre-oxidation for 2 hours, placing the fiber net in a high-temperature tube furnace, heating to 780 ℃ at a heating rate of 4 ℃ per minute under the protection of inert gas, preserving heat for 1.5 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorption material.
Comparative example 3
A textile-based oil absorbing material, made by the method comprising:
S1, mixing a multi-wall carbon nano tube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under ice bath conditions (the frequency is 38kHz, the power is 550W, the treatment time is 2.5 h) to form a homogeneous suspension, wherein the mass ratio of the multi-wall carbon nano tube, the modified Fe 3O4 powder to the sodium dodecyl benzene sulfonate aqueous solution is 2:1:50, and the sodium dodecyl benzene sulfonate in the sodium dodecyl benzene sulfonate aqueous solution accounts for 0.4% of the total mass of the multi-wall carbon nano tube and the modified Fe 3O4 powder;
The preparation method of the modified Fe 3O4 powder comprises the steps of taking cyclohexane, adding nonylphenol polyoxyethylene ether accounting for 0.06% of the cyclohexane volume, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of hexamethyldisilazane accounting for 4% of the cyclohexane volume and the concentration of 0.6mol/L into the emulsion, stirring and reacting to obtain Fe 3O4 particle dispersion, dropwise adding tetraethoxysilane accounting for 18% of the cyclohexane volume and ammonia water accounting for 2mol/L of the cyclohexane volume into the Fe 3O4 particle dispersion, stirring and reacting to obtain Fe 3O4 composite particles with surface coated silicon dioxide, separating and taking Fe 3O4 composite particles, adding 1g of particles into ethanol according to the proportion of 55mL of ethanol, heating to 58 ℃ and stirring uniformly, then adding hexamethyldisilazane accounting for 14% of the ethanol volume, heating to 125 ℃ and stirring and reacting for 2h, separating and taking 3O4 composite particles, washing and drying to obtain modified Fe 3O4 powder, and obtaining spherical powder with a transmission electron microscope (JEM 1200- 3O4) which has obvious characteristics, wherein the appearance is shown by the graph, and the appearance of the spherical powder is not shown by the graph, and the appearance of the spherical powder is obtained.
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment (the pressure is-0.1 MPa and the time is 2.5 h) to obtain an electrostatic spinning solution, wherein the mass ratio of the polyacrylonitrile fibers to the N, N-dimethylformamide to the suspension to the polydimethylsiloxane hydrophobic modifier to the dibutyltin dilaurate catalyst in the electrostatic spinning solution is 11:95:2.5:0.8:0.012;
S3, carrying out electrostatic spinning to form a net by using the electrostatic spinning solution, wherein the electrostatic spinning voltage is 20kV, the liquid supply speed is 3mL/h, the receiving distance is 15cm, the inner diameter of a needle head is 0.4mm, the rotating speed of a dynamic receiving aluminum roller is 30rpm, a fiber net is obtained, the thousand-worm shell powder accounting for 6% of the fiber net mass is uniformly sprayed on the surface of the fiber net, the fiber net is heated to 115 ℃ and maintained for 7S, and the fiber net is softened and combined with the thousand-worm shell powder;
The preparation method of the Qianchu insect shell powder comprises cleaning artificially cultured Qianchu insect, removing impurities, lyophilizing, and pulverizing to obtain shell powder with particle diameter of about 70 μm to obtain Qianchu insect shell powder;
S4, placing the fiber net in an air atmosphere at 275 ℃ for pre-oxidation for 2 hours, placing the fiber net in a high-temperature tube furnace, heating to 780 ℃ at a heating rate of 4 ℃ per minute under the protection of inert gas, preserving heat for 1.5 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorption material.
3. Performance testing
(1) Surface wettability
The oil absorbing material samples prepared in examples 1 to 3 and comparative examples 1 to 3 were taken, photographs of the droplets (5. Mu.L of deionized water droplets and 5. Mu.L of crude oil droplets taken with an instrument) when they contacted the surface of the oil absorbing material sample were taken using a video contact angle meter (DSA-20), and the contact angle of the droplets when they contacted the oil absorbing material sample was calculated using Image pro software.
(2) Oil absorption properties
And (3) absorbing oil at normal temperature, namely taking the textile-based oil absorption material samples prepared in the examples 1-3 and the comparative examples 1-3, respectively weighing the initial mass of the material samples, soaking the material samples on the surface of simulated viscous oil (prepared by seawater and crude oil according to the volume ratio of 7:3), performing static absorption, taking out the material samples after 5 minutes, and then retaining the material samples in the air for 30 seconds to enable excessive crude oil to drop under the action of self gravity, respectively weighing the absorbed mass, and calculating the oil absorption multiplying power by referring to the following formula. Repeating the steps for three times, and taking the average value of the results of the three times as the final oil absorption multiplying power result.
Wherein m0 is the initial mass, g is the mass after oil absorption, and m1 is g is the mass after oil absorption.
Photo-thermal oil absorption the textile-based oil absorption materials prepared in examples 1-3 and comparative examples 1-3 were taken, the temperature was raised under the irradiation of sunlight, the real-time temperature was recorded by a contact thermocouple (TES-1384) in real time, the photo-thermal properties were evaluated, and the oil absorption rate test was conducted again with reference to the above method when the sunlight was irradiated for 10 min. The sunlight irradiation is provided by a simulated sunlight xenon lamp light source (CEL-PE 300-4A, manufactured by the technology Co., ltd.) and is combined with an optical power densitometer, and the light intensity is controlled by adjusting the voltage (1.0 sun standard sunlight intensity).
4. Analysis of results
(1) Surface wettability
The photographs of the textile-based oil absorbing materials prepared in examples 1 to 3 and comparative examples 1 to 3 at the contact surface of the water droplets are shown in fig. 2, and the photographs of the textile-based oil absorbing materials prepared in examples 1 to 3 and comparative examples 1 to 3 at the contact surface of the oil droplets are shown in fig. 3. It can be seen that the textile-based oil absorption materials prepared in examples 1-3 of the invention have excellent hydrophobic oil absorption performance, the water contact angle reaches over 149.6 degrees, and the oil contact angles are all 0 degrees. Comparative examples 1 to 3 were all adjustments based on example 2, in which comparative example 1 did not coat the Fe 3O4 powder with a thin layer of silica and the hexamethyldisilazane surface treatment, the hydrophobic and oil absorption properties were slightly reduced, the analysis was probably due to some influence of its sedimentation agglomeration on the material, comparative example 2 did not load the modified euphorbia shell powder on the surface of the web, the hydrophobic and oil absorption properties were significantly reduced, the water contact angle was reduced to 113.4 °, the oil contact angle was increased to 65.4 °, and comparative example 3 replaced the modified euphorbia shell powder with a normal euphorbia shell powder, the hydrophobic and oil absorption properties were also significantly reduced, the water contact angle was reduced to 123.7 °, and the oil contact angle was increased to 41.3 °. Therefore, the modified Qianchu insect shell powder plays an important role in promoting the hydrophobic oil absorption performance of the material.
(2) Oil absorption properties
The oil absorption ratio results of the textile-based oil absorption materials prepared in examples 1 to 3 and comparative examples 1 to 3 were statistically obtained as shown in the following table 1:
TABLE 1 oil absorption multiplying power of each group of textile-based oil absorption materials for absorbing oil at normal temperature and absorbing oil by photo-thermal
As can be seen from the above Table 1, the textile-based oil absorption material prepared by the invention has outstanding oil absorption performance, especially in example 2, the oil absorption multiplying power at normal temperature reaches 45.14g/g, and the photo-thermal oil absorption multiplying power reaches 62.17g/g. In comparative example 1, the oil absorption performance of the Fe 3O4 powder is slightly reduced compared with that of example 2, but the photo-thermal oil absorption rate is obviously reduced, so that the modification treatment of the Fe 3O4 powder can obviously improve the photo-thermal performance of the Fe 3O4 powder, in comparative example 2, the surface of the fiber net is not loaded with modified euphorbia shell powder, the oil absorption rates of the modified euphorbia shell powder are obviously reduced compared with that of example 2 by 21.6% and 18.7%, in comparative example 3, the modified euphorbia shell powder is replaced by common euphorbia shell powder, the oil absorption rates of the modified euphorbia shell powder at normal temperature and photo-thermal are also obviously reduced compared with that of example 2 by 11.1% and 12.6%, and the oil absorption performance of the modified euphorbia shell powder on the material is further obviously improved.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.

Claims (8)

1. A textile-based oil absorbing material, characterized in that it is produced by the following method:
S1, mixing a multiwall carbon nanotube with modified Fe 3O4 powder, adding a sodium dodecyl benzene sulfonate aqueous solution, and performing ultrasonic treatment under an ice bath condition to form a homogeneous suspension;
the preparation method of the modified Fe 3O4 powder comprises the following steps:
adding polyoxyethylene nonylphenol ether accounting for 0.04-0.08% of the volume of cyclohexane into cyclohexane, stirring and dispersing uniformly to obtain emulsion, then dropwise adding an aqueous solution of ferric chloride hexahydrate accounting for 3-5% of the volume of cyclohexane and having the concentration of 0.4-0.8mol/L and ammonia accounting for 6-8% of the volume of cyclohexane and having the concentration of 1.5-2.5mol/L into the emulsion, and stirring and reacting to obtain Fe 3O4 particle dispersion;
Dripping ethyl orthosilicate accounting for 16-20% of the volume of cyclohexane and ammonia water accounting for 15-20% of the volume of cyclohexane and having the concentration of 1.5-2.5mol/L into the Fe 3O4 particle dispersion liquid, and stirring and reacting to obtain Fe 3O4 composite particles with the surfaces coated with silicon dioxide;
Separating Fe 3O4 composite particles, adding the composite particles into ethanol according to the proportion of 1g of the particles to 50-60mL of ethanol, heating to 55-60 ℃ and uniformly stirring, adding hexamethyldisilazane accounting for 12-16% of the volume of the ethanol, heating to 120-130 ℃ and stirring for reacting for 1.5-2.5h;
Separating Fe 3O4 composite particles, and cleaning and drying to obtain modified Fe 3O4 powder;
S2, adding polyacrylonitrile fibers into N, N-dimethylformamide, stirring until the polyacrylonitrile fibers are completely dissolved, adding the suspension, continuously stirring and dripping a polydimethylsiloxane hydrophobic modifier and a dibutyltin dilaurate catalyst, and carrying out vacuum defoaming treatment to obtain an electrostatic spinning solution;
S3, carrying out electrostatic spinning and net forming by using the electrostatic spinning solution to obtain a fiber net, uniformly spraying modified euphorbia shell powder accounting for 4-8% of the fiber net to the surface of the fiber net, heating the fiber net to 110-120 ℃ and maintaining for 6-8S, so that the fiber net is softened and combined with the modified euphorbia shell powder;
The preparation method of the modified Qianchu insect shell powder comprises the steps of cleaning artificially cultured Qianchu insect, removing impurities, soaking in 0.3-0.5M HCl solution for 0.5-1.5h, taking out, freeze-drying and crushing to obtain shell powder, soaking the shell powder in ethanol solution containing 8-12wt% of ethyl orthosilicate for 1.5-2h, taking out the shell powder, solidifying at 50-60 ℃ for 8-12h, soaking the shell powder in acetic acid solution containing 1.5-2wt% of chitosan and 0.8-1.2wt% of boric acid, stirring for reacting at 50-60 ℃ for 2-4h, finally taking out the shell powder, washing with water and drying to obtain the modified Qianchu insect shell powder;
S4, placing the fiber net in an air atmosphere at 270-280 ℃ for pre-oxidation for 1.5-2.5 hours, placing the fiber net in a high-temperature tube furnace, heating to 750-800 ℃ at a heating rate of 3-5 ℃ per minute under the protection of inert gas, preserving heat for 1-2 hours, and finally naturally cooling to room temperature to obtain the textile-based oil absorbing material.
2. The textile-based oil absorbing material according to claim 1, wherein in the step S1, the mass ratio of the multiwall carbon nanotubes to the modified Fe 3O4 powder to the aqueous solution of sodium dodecyl benzene sulfonate is 1-3:0.5-1.5:50, and sodium dodecyl benzene sulfonate accounts for 0.3-0.5% of the total mass of the multiwall carbon nanotubes and the modified Fe 3O4 powder.
3. The textile-based oil absorbing material of claim 1, wherein in step S1, the ultrasonic treatment is performed at a frequency of 35-40kHz, a power of 500-600W, and a treatment time of 2-3h.
4. The textile-based oil absorbing material according to claim 1, wherein in step S2, the mass ratio of polyacrylonitrile fiber, N-dimethylformamide, suspension, polydimethylsiloxane hydrophobic modifier and dibutyltin dilaurate catalyst in the electrostatic spinning solution is 10-12:90-100:2-3:0.8-0.9:0.01-0.015.
5. The textile-based oil absorbing material according to claim 1, wherein in step S2, the vacuum defoaming treatment is performed at a pressure of-0.1 MPa for a time of 2 to 3 hours.
6. The textile-based oil absorbing material according to claim 1, wherein in the step S3, the voltage of the electrostatic spinning is 15-25kV, the liquid supply speed is 2-4mL/h, the receiving distance is 12-18cm, the inner diameter of the needle is 0.3-0.5mm, and the rotating speed of the dynamic receiving aluminum roller is 10-50rpm.
7. A textile-based oil absorbing material as claimed in claim 1, wherein the shell powder has a particle size of 60-80 μm.
8. Use of the textile-based oil absorbing material of any one of claims 1-7 in heavy oil photothermal absorption.
CN202511090789.9A 2025-08-05 2025-08-05 Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption Active CN120586830B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202511090789.9A CN120586830B (en) 2025-08-05 2025-08-05 Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202511090789.9A CN120586830B (en) 2025-08-05 2025-08-05 Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption

Publications (2)

Publication Number Publication Date
CN120586830A CN120586830A (en) 2025-09-05
CN120586830B true CN120586830B (en) 2025-10-24

Family

ID=96884406

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202511090789.9A Active CN120586830B (en) 2025-08-05 2025-08-05 Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption

Country Status (1)

Country Link
CN (1) CN120586830B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106268659A (en) * 2016-04-21 2017-01-04 浙江海洋学院 A kind of industrial waste water purifying agent and preparation method thereof
CN120502243A (en) * 2025-07-07 2025-08-19 山西大学 Preparation method and application of photo-thermal dual-response film material

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4636869B2 (en) * 2004-12-21 2011-02-23 日揮触媒化成株式会社 Method for producing porous silica-based particles and porous silica-based particles obtained from the method
US20190015815A1 (en) * 2016-03-06 2019-01-17 Waters Technologies Corporation Superficially porous materials comprising a coated core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations
CN109853086B (en) * 2018-11-08 2021-09-03 大连工业大学 Lignin/cellulose acetate based electrostatic spinning carbon fiber and preparation method and application thereof
CN118206150A (en) * 2024-03-11 2024-06-18 湖南工程学院 A method for preparing La(OH)3 and La2O3 by electrospinning
CN119877149A (en) * 2025-01-23 2025-04-25 中国地质大学（北京） Core-shell structure photo-thermal phase change fiber material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106268659A (en) * 2016-04-21 2017-01-04 浙江海洋学院 A kind of industrial waste water purifying agent and preparation method thereof
CN120502243A (en) * 2025-07-07 2025-08-19 山西大学 Preparation method and application of photo-thermal dual-response film material

Also Published As

Publication number Publication date
CN120586830A (en) 2025-09-05

Similar Documents

Publication Publication Date Title
CN106744831B (en) A kind of reusable redox graphene base photothermal conversion film and its preparation method
CN111013503B (en) A kind of liquid metal aerogel, its preparation method and application
CN105001846B (en) A kind of fine and close oily waterflooding extraction increasing injection nano fluid and preparation method and application
CN109096998B (en) A kind of preparation method of photothermal conversion phase change energy storage composite material
CN102515145A (en) Preparation process for high specific surface porous carbon material
CN107254068B (en) A kind of carbon nano tube flexible conduction aeroge and preparation method thereof with water sensing function
Rong et al. MOFs meets wood: Renewable, self-supporting carbon-based composites for electromagnetic interference shielding with heat-resistant and electrothermal management
CN107384318B (en) Application of inorganic nano material in dust suppression
CN112786855B (en) Pomegranate-like structure silicon-carbon composite material, preparation method and application thereof
CN103400701B (en) A kind of manganese dioxide/carbon nanotube composite material and preparation method thereof
CN103723705A (en) Graphene/nano-aluminum compound and preparation method thereof
CN114849599A (en) A kind of nanocellulose composite carbon aerogel ball and its preparation method and application
CN113070043A (en) Super-hydrophobic cotton material with photo-thermal effect and preparation method and application thereof
CN103569989B (en) Preparation method and application of a Co3(PO4)2 microsphere flower-like hierarchical structure three-dimensional electrode material
CN114672184A (en) A kind of ultra-black light absorbing coating and preparation method and application thereof
CN112187109A (en) Preparation method of functional array for hydroelectric generator
CN107447292B (en) A kind of preparation method of micro-nano spiral porous fiber and its application
CN120586830B (en) Textile-based oil absorption material and application thereof in heavy oil photo-thermal absorption
CN113318700A (en) Porous cellucotton and preparation method and application thereof
CN114853453B (en) A kind of micronano structured hydrophobic ceramic airgel material and its preparation method
CN105702484B (en) A kind of preparation method of the mesoporous Nano carbon balls of electrode material for super capacitor NiO/
CN108183038A (en) A kind of preparation method of high specific capacitance Low ESR Graphene/carbon nanotube composite material
CN113135558B (en) Photothermal material based on porous carbon spheres and preparation method thereof
CN103395773B (en) Nano carbon hollow sphere and preparation method thereof
CN114944480A (en) Preparation method of honeycomb porous tin-carbon composite material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant