CN113070043A - Super-hydrophobic cotton material with photo-thermal effect and preparation method and application thereof - Google Patents
Super-hydrophobic cotton material with photo-thermal effect and preparation method and application thereofDownload PDFInfo
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- CN113070043A CN113070043ACN202110254424.0ACN202110254424ACN113070043ACN 113070043 ACN113070043 ACN 113070043ACN 202110254424 ACN202110254424 ACN 202110254424ACN 113070043 ACN113070043 ACN 113070043A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
Translated fromChinese
Description
Technical Field
The invention relates to the field of preparation of oil-water separation materials, in particular to a super-hydrophobic cotton material with a photothermal effect, and a preparation method and application thereof.
Background
Petroleum has been an essential part of society as an energy source for over a century. However, in the last decade, oil spill accidents and petroleum-polluted industrial wastewater cause serious environmental pollution, which affects the living environment of aquatic animals and the ecological balance of the whole water body. In order to maintain ecological balance and make full use of oil spills, researchers have proposed various methods to prepare a series of adsorbent materials to remove or recover oil spills and waste water. The cotton-based material is a natural material, has the advantages of economy, environmental protection, strong adsorbability, easy modification and the like, and is widely applied to the field of oil-water separation. However, when these materials face the leakage of the offshore oil, the adsorption material has poor adsorption performance on the high-viscosity crude oil, and the recovery rate is low, which becomes a difficult problem of the recovery of the oil leakage.
The viscosity of the crude oil is in a negative correlation with the temperature, and when the temperature is lower than 60 ℃, the viscosity of the crude oil is lower than 0.1 (pa · s), and good fluidity is shown. This motivates researchers to assist in oil-water separation by preparing materials that can be heated. However, these methods have the disadvantages of complicated steps, expensive raw materials, additional energy requirement, etc. Solar energy is an inexhaustible energy source, which enables the photothermal conversion material to be widely applied. Carbon Nanotubes (CNTs) are widely used due to their broad band of light absorption and chemical stability, and demonstrate high light-to-heat conversion efficiency. In addition, the irregular, rough microstructure of the carbon nanotubes makes it easy to modify and form superhydrophobic surfaces. However, few materials have been prepared that combine carbon nanotubes with hydrophobic functional groups to prepare photothermal materials to treat high viscosity crude oil leakage.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a high-efficiency superhydrophobic cotton material with a photothermal effect, a preparation method and an application thereof, aims to solve the problem of leakage of high-viscosity crude oil, and overcomes the defects of the conventional superhydrophobic material in the process of separating heavy oil from water with high viscosity.
The technical scheme of the invention is as follows:
a method for preparing a super-hydrophobic cotton material with a photo-thermal effect comprises the following steps:
providing a cotton material;
pretreating the cotton material with ethanol;
dispersing polyhydroxy carbon nanotubes into ethanol, adding tetraethyl silicate and hexadecyl trimethoxy silane, and preparing super-hydrophobic nanoparticles;
dispersing the super-hydrophobic nano-particles into n-hexane to prepare a modified solution;
and immersing the pretreated cotton material into the modified solution, and drying to obtain the super-hydrophobic cotton material.
The preparation method of the super-hydrophobic cotton material with the photo-thermal effect comprises the following steps of preparing a cotton material, wherein the cotton material comprises but is not limited to non-woven fabrics, cotton fabrics or fabrics of cotton substrates.
The preparation method of the super-hydrophobic cotton material with the photo-thermal effect comprises the following steps of:
soaking the dried cotton material in ethanol solution at normal temperature for 5min, washing with deionized water, placing in oven, and drying at 60 deg.C for 8 h.
The preparation method of the superhydrophobic cotton material with the photo-thermal effect comprises the following steps of:
dispersing polyhydroxy Carbon Nano Tubes (CNT) in ethanol, and adding ammonia water to prepare a first suspension;
adding a tetraethyl silicate (TEOS) -ethanol mixed solution into the first suspension, and carrying out ultrasonic treatment for 2h to prepare a second suspension;
adding hexadecyl trimethoxy silane (HDTMS) to the second suspension, and performing ultrasonic treatment for 1h to prepare a third suspension;
and centrifuging the third suspension, and washing with ethanol to prepare the super-hydrophobic nano-particles.
The preparation method of the superhydrophobic cotton material with the photo-thermal effect comprises the following steps: the inner diameter is 2-5nm, the outer diameter is less than 8nm, and the length is 10-30 μm.
The preparation method of the superhydrophobic cotton material with the photo-thermal effect comprises the step of preparing tetraethyl silicate-ethanol mixed solution, wherein the volume ratio of tetraethyl silicate to ethanol in the tetraethyl silicate-ethanol mixed solution is 1: 5.
The preparation method of the super-hydrophobic cotton material with the photo-thermal effect comprises the following steps of: and (3) dispersing dimethyl Polysiloxane (PDMS), a curing agent and the super-hydrophobic nano particles in n-hexane, and performing ultrasonic treatment for 1h to prepare the modified solution.
The preparation method of the super-hydrophobic cotton material with the photo-thermal effect comprises the step of preparing a super-hydrophobic cotton material with the photo-thermal effect, wherein the mass ratio of dimethyl Polysiloxane (PDMS) to a curing agent is 10: 1.
A super-hydrophobic cotton material with a photo-thermal effect is prepared by adopting the preparation method.
The application of the super-hydrophobic cotton material with the photo-thermal effect is characterized in that the super-hydrophobic cotton material with the photo-thermal effect is used for oil-water separation.
Has the advantages that: the invention adheres the super-hydrophobic nano-particles on the fiber of the cotton material to obtain the super-hydrophobic cotton material with the photo-thermal effect: firstly, carrying out superhydrophobic modification on a polyhydroxy Carbon Nanotube (CNT), obtaining long-chain hydrophobic groups through hydrolysis and condensation reactions between TEOS and HDTMS loaded on the CNT, drying to obtain superhydrophobic nanoparticles, and adhering the superhydrophobic nanoparticles on a cotton material by utilizing excellent adhesiveness of PDMS to obtain the superhydrophobic cotton material with a photo-thermal effect. The super-hydrophobic cotton material prepared by the invention has excellent super-hydrophobic performance, can generate a photo-thermal effect under the illumination condition, has high adsorption efficiency on heavy oil with high viscosity, and can perform effective oil-water separation. In addition, the viscosity of the heavy oil is reduced through photothermal effect, and the adsorption and desorption efficiency of the heavy oil can be obviously improved. Meanwhile, the super-hydrophobic modified cotton material has excellent wear resistance, acid and alkali resistance and excellent separation efficiency on other oils except crude oil.
Drawings
Fig. 1 is a flow chart of a preferred embodiment of a method for preparing a superhydrophobic cotton material with a photo-thermal effect according to the present invention.
Fig. 2 is a flow chart of a preferred embodiment of a method for preparing superhydrophobic nanoparticles according to the present invention.
Fig. 3 is a schematic diagram of a process for forming superhydrophobic nanoparticles according to the present invention.
FIG. 4 is a data graph showing the oil-water separation efficiency of the superhydrophobic cotton material under the presence or absence of sunlight for various organic solvents and oils (n-pentane, n-hexane, n-octane, dodecane, 1, 2-dichloroethane, Tween 80, crude oil) in example 1.
Detailed Description
The invention provides a super-hydrophobic cotton material with a photothermal effect, and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, a flow chart of a preferred embodiment of a method for preparing a superhydrophobic cotton material having a photo-thermal effect according to an embodiment of the present invention is shown in the figure, and includes the following steps:
s10, providing a cotton material;
s20, pretreating the cotton material with ethanol;
s30, dispersing the polyhydroxy carbon nano-tube (CNT) into ethanol, adding tetraethyl silicate (TEOS) and hexadecyl trimethoxy silane (HDTMS) to prepare super-hydrophobic nano-particles;
s40, dispersing the super-hydrophobic nano particles into n-hexane to prepare a modified solution;
and S50, immersing the pretreated cotton material into the modified solution, and drying to obtain the super-hydrophobic cotton material.
In some embodiments, the cotton material includes, but is not limited to, a non-woven fabric, a cotton fabric, or a fabric of cotton-based material.
In some embodiments, the step of subjecting the cotton material to ethanol pretreatment comprises: soaking the dried cotton material in ethanol solution at normal temperature for 5min, washing with deionized water, placing in oven, and drying at 60 deg.C for 8 h.
In some embodiments, the step of preparing the superhydrophobic nanoparticle is shown in fig. 2 and comprises:
s301, dispersing polyhydroxy Carbon Nanotubes (CNT) in ethanol, and adding ammonia water to prepare a first suspension;
s302, adding a tetraethyl silicate (TEOS) -ethanol mixed solution into the first suspension, and carrying out ultrasonic treatment for 2 hours to prepare a second suspension;
s303, adding hexadecyl trimethoxy silane (HDTMS) into the second suspension, and carrying out ultrasonic treatment for 1h to prepare a third suspension;
s304, centrifuging the third suspension, and washing with ethanol to prepare the super-hydrophobic nano-particles.
In some specific embodiments, the polyhydroxy carbon nanotubes have dimensions of: 95%, an inner diameter of 2-5nm, an outer diameter <8nm, and a length of 10-30 μm, but is not limited to this dimension.
In some specific embodiments, the volume ratio of tetraethyl silicate (TEOS) to ethanol in the tetraethyl silicate (TEOS) -ethanol mixed solution is 1: 5.
In some specific embodiments, the superhydrophobic modifier includes, but is not limited to, Hexadecyltrimethoxysilane (HDTMS).
In some embodiments, the step of preparing the modifying solution comprises: and (3) dispersing dimethyl Polysiloxane (PDMS), a curing agent and the super-hydrophobic nano particles in n-hexane, and performing ultrasonic treatment for 1h to prepare the modified solution.
In some specific embodiments, the mass ratio of the dimethylpolysiloxane (PDMS) to the curing agent is 10: 1.
The invention also provides a super-hydrophobic cotton material with a photo-thermal effect, wherein the super-hydrophobic cotton material is prepared by adopting any one of the preparation methods.
The invention obtains the super-hydrophobic cotton material with the photo-thermal effect by adhering the super-hydrophobic nano particles to the fibers of the cotton material, wherein the cotton material is essentially water-absorbent. The high-efficiency super-hydrophobic cotton material prepared by the invention generates a photo-thermal effect under the illumination condition, has high adsorption efficiency on heavy oil with high viscosity, and can perform effective oil-water separation. And the viscosity of the heavy oil is reduced through the photothermal effect, and the adsorption and desorption efficiency of the heavy oil can be obviously improved. Meanwhile, the modified cotton material has excellent wear resistance, acid and alkali resistance and excellent separation efficiency for other oils except crude oil.
Specifically, referring to fig. 3, in this embodiment, a superhydrophobic modification is performed on a polyhydroxy carbon nanotube, a long-chain hydrophobic group is obtained through hydrolysis and condensation reactions between TEOS and HDTMS loaded on a CNT, and the superhydrophobic nanoparticle is obtained by drying the hydrophobic group. And adhering the PDMS on a cotton material by utilizing the excellent adhesiveness of PDMS to obtain the super-hydrophobic cotton material with photo-thermal properties. The super-hydrophobic cotton material prepared by the embodiment has excellent super-hydrophobic performance and photo-thermal effect. In the face of ocean oil leakage and other similar events, when the super-hydrophobic cotton material is exposed to the sun, the viscosity of heavy oil adsorbed on the cotton material can be reduced due to the temperature rise of the cotton material caused by the photo-thermal effect, and the desorption of crude oil on the cotton material and the reutilization property of the modified cotton material are facilitated. Meanwhile, the modified cotton material has excellent abrasion resistance, acid and alkali resistance and excellent separation efficiency for other oils except crude oil.
The invention also discloses application of the super-hydrophobic cotton material with the photo-thermal effect, and the super-hydrophobic cotton material with the photo-thermal effect is used for oil-water separation.
The following is a further explanation of the super-hydrophobic cotton material with photothermal effect, its preparation method and application by specific examples:
example 1
Preparation of super-hydrophobic cotton material with photothermal effect
(1) Providing a cotton material, soaking the dried cotton material in an ethanol solution at normal temperature for 5min, then washing with a large amount of deionized water, and putting into an oven for drying for 8h at 60 ℃.
(2) Dispersing 0.2g of CNT (polyhydroxy carbon nanotube) in 50ml of ethanol, and dropwise adding 3ml of ammonia water; a TEOS (tetraethyl silicate) -ethanol mixed solution (2 mL of TEOS, 10 mL of ethanol) is slowly injected into the suspension and kept for 2h under ultrasonic treatment; 2.3mL of HDTMS (hexadecyltrimethoxysilane) was added dropwise to the above solution, followed by sonication for 1 h; the resulting solution was centrifuged at 10000rpm/min for 20 minutes and washed several times with ethanol to finally obtain superhydrophobic nanoparticles, noted as CNT @ TEOS/HDTMS particles.
(3) 2g of CNT @ TEOS/HDTMS particles, 2g of PDMS and 0.2g of a curing agent were dispersed in 150ml of n-hexane to obtain a modified solution, and subjected to ultrasonic treatment for 1 hour.
(4) And (3) immersing the dried cotton material treated by the ethanol into the modified solution for 1h, taking out, waiting for the solvent to volatilize at room temperature, and drying at 80 ℃ for 8h to obtain the super-hydrophobic modified cotton material.
Performance testing of superhydrophobic cotton materials with photothermal effect
(1) Oil-water separation efficiency test
Respectively carrying out oil-water separation test on the super-hydrophobic modified cotton material prepared in the example 1 and the crude cotton-oil mixture prepared in the comparative example 1, wherein the oil phase is selected from crude oil, a xenon lamp is utilized to simulate solar illumination, and the light intensity is 1kw/m2。
Taking 5ml of crude oil and 95ml of pure water mixed solution as an oil-water mixture, taking a cotton material in the form of an oil skimmer as a separation vessel to perform oil-water separation test, and calculating the oil-water separation efficiency according to a formula:
(m0representing the mass of water before oil-water separation, m1Representing the quality of water after oil-water separation)
As can be seen from fig. 4, under the same test conditions, the oil-water separation efficiency of the superhydrophobic cotton material can reach 98%, and the original cotton can not achieve the oil-water separation effect because it absorbs both water and oil.
In summary, the invention provides a superhydrophobic cotton material with a photo-thermal effect, which is prepared by performing superhydrophobic modification on a polyhydroxy Carbon Nanotube (CNT), obtaining long-chain hydrophobic groups through hydrolysis and condensation reactions between TEOS and HDTMS loaded on the CNT, and drying to obtain superhydrophobic nanoparticles. And adhering the PDMS on a cotton material by utilizing the excellent adhesiveness of PDMS to obtain the super-hydrophobic cotton material with photo-thermal properties. The super-hydrophobic cotton material prepared by the invention not only has excellent super-hydrophobic performance, but also has photo-thermal effect, can generate photo-thermal effect under illumination condition, has high adsorption efficiency on heavy oil with high viscosity, and can perform effective oil-water separation; in addition, the viscosity of the heavy oil is reduced through the photothermal effect, and the adsorption and desorption efficiency of the heavy oil can be obviously improved; meanwhile, the modified cotton material has excellent wear resistance, acid and alkali resistance and excellent separation efficiency for other oils except crude oil.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a super-hydrophobic cotton material with a photothermal effect is characterized by comprising the following steps:
providing a cotton material;
pretreating the cotton material with ethanol;
dispersing polyhydroxy carbon nanotubes into ethanol, adding tetraethyl silicate and hexadecyl trimethoxy silane, and preparing super-hydrophobic nanoparticles;
dispersing the super-hydrophobic nano-particles into n-hexane to prepare a modified solution;
and immersing the pretreated cotton material into the modified solution, and drying to obtain the super-hydrophobic cotton material.
2. The method of preparing a superhydrophobic cotton material having a photothermal effect according to claim 1, wherein the cotton material includes but is not limited to non-woven fabric, cotton fabric or cotton-based fabric.
3. The method for preparing superhydrophobic cotton material with photothermal effect according to claim 1, wherein the step of pretreating the cotton material with ethanol comprises:
soaking the dried cotton material in ethanol solution at normal temperature for 5min, washing with deionized water, placing in oven, and drying at 60 deg.C for 8 h.
4. The method for preparing superhydrophobic cotton material with photothermal effect according to claim 1, wherein the step of preparing superhydrophobic nanoparticles comprises:
dispersing the polyhydroxy carbon nano tube in ethanol, and adding ammonia water to prepare a first suspension;
adding a tetraethyl silicate-ethanol mixed solution into the first suspension, and carrying out ultrasonic treatment for 2 hours to prepare a second suspension;
adding hexadecyl trimethoxy silane into the second suspension, and carrying out ultrasonic treatment for 1h to prepare a third suspension;
and centrifuging the third suspension, and washing with ethanol to prepare the super-hydrophobic nano-particles.
5. The method for preparing superhydrophobic cotton material with photothermal effect according to claim 4, wherein the size of the polyhydroxy carbon nanotube is: the inner diameter is 2-5nm, the outer diameter is less than 8nm, and the length is 10-30 μm.
6. The method for preparing the superhydrophobic cotton material with the photothermal effect according to claim 4, wherein the volume ratio of the tetraethyl silicate to the ethanol in the tetraethyl silicate-ethanol mixed solution is 1: 5.
7. The method for preparing the superhydrophobic cotton material with the photothermal effect according to claim 1, wherein the step of preparing the modification solution comprises: and dispersing dimethyl polysiloxane, a curing agent and the super-hydrophobic nano particles in n-hexane, and performing ultrasonic treatment for 1h to prepare the modified solution.
8. The method for preparing the superhydrophobic cotton material with the photothermal effect according to claim 7, wherein the mass ratio of the dimethylpolysiloxane to the curing agent is 10: 1.
9. A superhydrophobic cotton material having a photothermal effect, prepared by the method of any one of claims 1-8.
10. Use of a superhydrophobic cotton material with a photothermal effect, wherein the superhydrophobic cotton material with a photothermal effect as claimed in claim 9 is used for oil-water separation.
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| CN116673010A (en)* | 2023-06-20 | 2023-09-01 | 河南大学 | A photothermal superhydrophobic porous material based on ultralight clay and its preparation method and application |
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| CN118994957A (en)* | 2024-08-13 | 2024-11-22 | 中国石油大学(华东) | DTMS@PDA@SiO2Nano CNTs composite material, preparation and application thereof, super-hydrophobic self-repairing anticorrosive paint and coating and preparation thereof |
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