CN112107887A - Underwater super-oleophobic oil-water separation material and preparation method and application thereof - Google Patents
Underwater super-oleophobic oil-water separation material and preparation method and application thereof Download PDFInfo
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- CN112107887A CN112107887A CN202010867126.4A CN202010867126A CN112107887A CN 112107887 A CN112107887 A CN 112107887A CN 202010867126 A CN202010867126 A CN 202010867126A CN 112107887 A CN112107887 A CN 112107887A
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- B01D17/02—Separation of non-miscible liquids
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Abstract
The invention belongs to the technical field of functional materials, and discloses an underwater super-oleophobic oil-water separation material, and a preparation method and application thereof. The method comprises the steps of soaking a mesh substrate in absolute ethyl alcohol, and then cleaning with deionized water; soaking the obtained mesh substrate in a sodium alginate solution; then soaking in calcium chloride solution; preparing a mesh substrate of the calcium alginate coating; and then washing the mesh-shaped substrate with the calcium alginate coating by using deionized water, repeatedly soaking the mesh-shaped substrate in a sodium alginate solution and a calcium chloride solution, and washing the mesh-shaped substrate with the deionized water to obtain the underwater superoleophobic oil-water separation material. The preparation process is simple and convenient, the material is suitable for various mesh substrates, the cost is low, the underwater super-oleophobic oil-water separation material can be used for oil-water separation of oil, acid and alkali systems for daily use, the oil-water separation effect is good, the material is environment-friendly and pollution-free, and the mesh substrate can be recycled.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to an underwater super-oleophobic oil-water separation material as well as a preparation method and application thereof.
Background
The oil-containing waste water discharged by petroleum leakage and industry not only threatens human life, but also has adverse effect on environment and ecology. Under such circumstances, the development of new advanced oil-water separation materials has become a priority in the industry and academia.
In recent years, oil-water separators which consume a large amount of energy have been developed in the industry. However, it has been found that gravity-driven grid separation may be an alternative, desirable method that has been widely used for low-cost oil-water separation. For example, an underwater super-oleophobic net with corrosion resistance and self-healing capability is made by the combination of a super-hydrophilic hydrogel and silica nanoparticles. While these materials have excellent superhydrophilic and superoleophobic properties, they still require complex manufacturing methods, expensive synthetic polymers, and non-biodegradable inorganic materials.
In order to solve the problems in practical application, a preparation method of a hydrogel-modified super-hydrophilic and underwater super-oleophobic material which is low in preparation cost, environment-friendly and biodegradable is urgently needed. Sodium alginate is a natural polysaccharide, has the stability, solubility, viscosity and safety required by pharmaceutical preparation accessories, and is widely applied in the food industry and the medical field. Sodium alginate can cross-link with polyvalent metal cations such as calcium ions to form a transparent gel having superhydrophilic/underwater superoleophobic properties.
Disclosure of Invention
In order to solve the defects of the prior art, a preparation method of an underwater super-oleophobic oil-water separation material is provided. The method has simple preparation process and low cost, the separation material can be used for oil-water separation of oil, acid and alkali systems for daily use, the oil-water separation effect is good, the material is environment-friendly and pollution-free, and the mesh substrate can be recycled.
The invention also aims to provide the underwater super-oleophobic oil-water separation material prepared by the method.
The invention further aims to provide application of the underwater super oleophobic oil-water separation material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an underwater super-oleophobic oil-water separation material comprises the following specific steps:
s1, soaking a mesh substrate in absolute ethyl alcohol, and then cleaning with deionized water;
s2, soaking the mesh-shaped substrate obtained in the step S1 in a sodium alginate solution, and then soaking the mesh-shaped substrate in a calcium chloride solution to obtain a mesh-shaped substrate with a calcium alginate coating;
and S3, washing the mesh-shaped substrate with the calcium alginate coating by using deionized water, repeating the step S2, and then washing by using the deionized water to obtain the underwater super-oleophobic oil-water separation material.
Preferably, the soaking time in the step S1 is 30-60S.
Preferably, in step S1, the mesh-shaped substrate is a metal mesh or a ceramic mesh, the metal mesh is a stainless steel mesh or a nickel mesh, and the pore size of the mesh-shaped substrate is 80-300 meshes.
Preferably, the sodium alginate solution in step S2 is prepared by dissolving sodium alginate in deionized water and performing ultrasonic cleaning.
More preferably, the volume ratio of the mass of the sodium alginate to the volume of the deionized water is (8-15) mg: 10 mL.
Preferably, the soaking time in the sodium alginate solution in the step S2 is 2-5 min; the time for soaking in the calcium chloride solution is 5-10 min.
Preferably, the calcium chloride solution in step S2 is prepared by dissolving anhydrous calcium chloride in deionized water and stirring, and the concentration of the calcium chloride solution is 5-10 wt%.
Preferably, the step S2 is repeated 2 to 3 times in the step S2.
An underwater super-oleophobic oil-water separation material is prepared by the method.
The underwater super-oleophobic oil-water separation material is applied to the fields of separation of oil-water mixtures, acid-base environments, applicability to hot water and cold water or treatment of oily sewage.
Compared with the prior art, the invention has the following beneficial effects:
1. the oil-water separation material disclosed by the invention has stable underwater super-oleophobic property for various oils (including edible vegetable oil), can be used for oil-water separation of acid, alkali, hot and cold systems, and is high in separation efficiency and good in oil-water separation effect.
2. The preparation process is simple and convenient, and the cost is low; the operation is simple, and the cleaning is easy; the material is environment-friendly and pollution-free, and the mesh substrate can be recycled.
Drawings
FIG. 1 is an underwater contact angle of soybean oil droplets on the oil-water separating material prepared in example 1.
FIG. 2 is a graph showing a static contact angle of water droplets on the oil-water separating material obtained in example 1.
FIG. 3 is an underwater contact angle of soybean oil droplets on the oil-water separating material prepared in example 2.
FIG. 4 is a graph showing a static contact angle of water droplets on the oil-water separating material obtained in example 2.
FIG. 5 is an underwater contact angle of various oils on the oil-water separating material prepared in example 3.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. Soaking a stainless steel net (100 meshes, the thickness is 10 mu m) in absolute ethyl alcohol for 30s, and cleaning the stainless steel net by using deionized water;
2. soaking the stainless steel net obtained in the step 1 in a sodium alginate solution of 108mg/100ml for 2 min; soaking in 5 wt% calcium chloride solution for 5min to obtain mesh substrate with calcium alginate coating;
3. and (3) washing the stainless steel mesh treated in the step (2) with deionized water, repeating the step (2) once, and then washing with deionized water to obtain the underwater super-oleophobic oil-water separation material.
FIG. 1 is an underwater contact angle of soybean oil droplets on the oil-water separating material prepared in example 1. As can be seen from FIG. 1, the obtained 4 data are averaged to obtain that the static contact angle of the oil on the surface of the stainless steel mesh in the water is greater than 150 degrees, the contact angle of the oil drop on the oil-water separation material is 153 degrees, and the prepared oil-water separation material is of an underwater super oleophobic structure. The static contact angle measurement of water droplets in the air was performed on the stainless steel net processed by the preparation method of example 1, and fig. 2 is a static contact angle of water droplets on the oil water separating material prepared in example 1. As can be seen from fig. 2, the contact angle of the water drop was measured at 4 different positions, the static contact angle of the water drop on the oil-water separation material was 0 °, and the oil-water separation material obtained was a superhydrophilic structure.
Example 2
1. Soaking a stainless steel net (150 meshes, the thickness of which is 10 mu m) in absolute ethyl alcohol for 30s, and cleaning the stainless steel net by using deionized water;
2. soaking the stainless steel mesh obtained in the step 1 in a 108mg/100ml sodium alginate solution for 2min, and then soaking in a 5 wt% calcium chloride solution for 5min to obtain a mesh substrate with a calcium alginate coating;
3. and (3) washing the stainless steel mesh treated in the step (2) with deionized water, repeating the step (2) twice, and washing with the deionized water to obtain the underwater super-oleophobic oil-water separation material.
The wettability of the surface of the stainless steel mesh processed by the preparation method of example 2 was tested. The surface of the stainless steel mesh processed by the preparation method of example 2 was subjected to the measurement of the static contact angle of the underwater oil, and the measurement of the static contact angle was performed using soybean oil droplets having a size of 10. mu.L. FIG. 3 is an underwater contact angle of soybean oil droplets on the oil-water separating material prepared in example 2. As can be seen from fig. 3, 4 different positions are measured on the sample, and the obtained 4 data are averaged to obtain that the static contact angle of the oil on the surface of the underwater stainless steel mesh is greater than 160 °, the prepared oil-water separation material is an underwater super-oleophobic structure, and fig. 4 is the static contact angle of the water droplet on the oil-water separation material prepared in example 2. As can be seen from fig. 4, 4 different positions are measured on the sample, and the average of the obtained 4 data is obtained to obtain a static contact angle of the water bead on the surface of the stainless steel net of 0 °.
The difference from example 1 is that: the mesh number of the stainless steel mesh is 150 meshes, the step 2 is repeated twice, the contact angle of water drops on the surface of the stainless steel mesh is 0 degrees, the static contact angle of underwater oil drops on the surface of the stainless steel mesh is 161 degrees, and the prepared oil-water separation material is of an underwater super-oleophobic/super-hydrophilic structure.
Example 3
1. Soaking a nickel net (100 meshes, the thickness is 10 mu m) in absolute ethyl alcohol for 30s, and cleaning the stainless steel net by using deionized water;
2. soaking the nickel screen obtained in the step 1 in a sodium alginate solution of 108mg/100ml for 2min, and then soaking in a calcium chloride solution of 5 wt% for 5min to obtain a mesh substrate of the calcium alginate coating;
3. and (3) washing the nickel screen treated in the step (2) with deionized water, repeating the step (2) twice, and washing with the deionized water to obtain the underwater super-oleophobic oil-water separation material.
The wettability of the surface of the nickel mesh processed by the preparation method of example 3 and the static contact angle of the oil under water on the surface of the nickel mesh were measured, the static contact angle was measured using soybean oil droplets of 10 μ L in size, 4 different positions were measured on the sample, and the obtained 4 data were averaged to obtain the static contact angle of the oil on the surface of the stainless steel mesh under water which was greater than 150 °. FIG. 5 is an underwater contact angle of various oils on the oil-water separating material prepared in example 3. As can be seen from FIG. 5, the underwater contact angles of a series of domestic oils (corn oil, soybean oil and peanut oil), n-hexadecane and dichloromethane in example 3 are all over 150 degrees, the dichloromethane is slightly soluble in water, and the contact angle also reaches 147 degrees, which proves that the prepared oil-water separation material has excellent underwater super-oleophobic property and can be applied to oil-water separation in water.
The difference from example 1 is that: the mesh-shaped substrate is a metal nickel mesh, the step 2 is repeated twice, the contact angle of water drops on the surface of the mesh-shaped substrate is 0 degrees, the static contact angle of underwater oil drops on the surface of the mesh-shaped substrate is 150 degrees, and the prepared oil-water separation material is of an underwater super-oleophobic/super-hydrophilic structure.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of an underwater super-oleophobic oil-water separation material is characterized by comprising the following specific steps:
s1, soaking a mesh substrate in absolute ethyl alcohol, and then cleaning with deionized water;
s2, soaking the mesh-shaped substrate obtained in the step S1 in a sodium alginate solution, and then soaking the mesh-shaped substrate in a calcium chloride solution to obtain a mesh-shaped substrate with a calcium alginate coating;
and S3, washing the mesh-shaped substrate with the calcium alginate coating by using deionized water, repeating the step S2, and then washing by using the deionized water to prepare the underwater super-oleophobic oil-water separation material.
2. The preparation method of the underwater superoleophobic oil-water separation material according to claim 1, characterized in that the soaking time in the step S1 is 30-60S.
3. The preparation method of the underwater superoleophobic oil-water separation material according to claim 1, characterized in that in step S1, the mesh-shaped substrate is a metal mesh or a ceramic mesh, the metal mesh is a stainless steel mesh or a nickel mesh, and the pore size of the mesh-shaped substrate is 80-300 meshes.
4. The preparation method of the underwater superoleophobic oil-water separation material according to claim 1, characterized in that the sodium alginate solution in step S2 is prepared by dissolving sodium alginate in deionized water and performing ultrasonic cleaning.
5. The preparation method of the underwater super-oleophobic oil-water separation material according to claim 4, characterized in that the volume ratio of the mass of sodium alginate to deionized water is (8-15) mg: 10 mL.
6. The preparation method of the underwater super-oleophobic oil-water separation material according to claim 1, characterized in that the soaking time in the sodium alginate solution in step S2 is 2-5 min; the time for soaking in the calcium chloride solution is 5-10 min.
7. The preparation method of the underwater super-oleophobic oil-water separation material according to claim 1, characterized in that the calcium chloride solution in step S2 is prepared by dissolving anhydrous calcium chloride in deionized water and stirring, and the concentration of the calcium chloride solution is 5-10 wt%.
8. The preparation method of the underwater superoleophobic oil-water separation material according to claim 1, characterized in that the number of times of repeating the step S2 in the step S2 is 2-3.
9. An underwater superoleophobic oil-water separation material, characterized in that the oil-water separation material is prepared by the method of any one of claims 1-8.
10. The underwater superoleophobic oil-water separation material of claim 9 is applied to the fields of separation of oil-water mixtures, acid-base environments, applicability to hot water and cold water or treatment of oily sewage.
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| CN202010867126.4A CN112107887A (en) | 2020-08-26 | 2020-08-26 | Underwater super-oleophobic oil-water separation material and preparation method and application thereof |
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| CN202010867126.4A CN112107887A (en) | 2020-08-26 | 2020-08-26 | Underwater super-oleophobic oil-water separation material and preparation method and application thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106853296A (en) * | 2016-12-30 | 2017-06-16 | 福建农林大学 | A kind of oil water separation type sodium alginate/graphene oxide composite aerogel and preparation method thereof |
| CN107185414A (en) * | 2017-06-01 | 2017-09-22 | 江苏大学 | A kind of graphene oxide/calcium alginate gel is modified the preparation method and its usage of composite membrane |
| CN107261862A (en) * | 2017-06-01 | 2017-10-20 | 江苏大学 | A kind of bat calcium alginate gel compound is modified the preparation method and its usage of composite membrane |
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- 2020-08-26 CN CN202010867126.4A patent/CN112107887A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106853296A (en) * | 2016-12-30 | 2017-06-16 | 福建农林大学 | A kind of oil water separation type sodium alginate/graphene oxide composite aerogel and preparation method thereof |
| CN107185414A (en) * | 2017-06-01 | 2017-09-22 | 江苏大学 | A kind of graphene oxide/calcium alginate gel is modified the preparation method and its usage of composite membrane |
| CN107261862A (en) * | 2017-06-01 | 2017-10-20 | 江苏大学 | A kind of bat calcium alginate gel compound is modified the preparation method and its usage of composite membrane |
Non-Patent Citations (1)
| Title |
|---|
| WANG, YAQUAN等: "A green strategy for preparing durable underwater superoleophobic calcium alginate hydrogel coated-meshes for oil/water separation", 《INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES》 * |
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