CN112057900B - Preparation method of oil-water separation material with excellent stability - Google Patents
Preparation method of oil-water separation material with excellent stability Download PDFInfo
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Abstract
The invention relates to a preparation method of an oil-water separation material with excellent stability, which comprises the following steps: placing 4 cm × 4 cm cotton cloth in 30ml absolute ethanol solution, ultrasonically washing and drying for later use, dissolving 0.3 ml KH570 coupling agent (gamma-methacryloxypropyltrimethoxysilane) in 20 ml deionized water and 2 ml ammonia water solution, placing the cotton cloth in the solution, and stirring at 60 ℃ for 6 hours to obtain KH570 grafted cotton cloth; placing the KH570 grafted cotton cloth in a beaker, stirring, adding 0.3 g of SBMA ([2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide) and 0.01 g of AIBN initiator, initiating a free radical polymerization reaction on the surface of the cotton cloth, stirring for 6 hours at 60 ℃, wherein the prepared modified cotton cloth still has good stability under the complex environment of strong acid and strong alkali, the application range of the material is expanded, and a good foundation is laid for the large-scale application of oil-water separation sponge.
Description
Technical Field
The invention relates to a preparation method of an oil-water separation material with excellent stability, and belongs to the technical field of super-hydrophobic oil-water separation.
Background
In recent years, with the rapid development of industrialization, oil-water pollution is more and more serious, especially, the oil pollutants in water and crude oil leakage seriously harm ecological balance and destroy social environment, such as crude oil leakage in gulf of mexico and oil spill in welfare oil field in usa, so that the problem of solving oil spill pollution becomes a problem which people have to pay attention to is solved, according to incomplete statistics, the global economic loss caused by the destruction of marine ecological environment every year is as high as 130, and about 92% of the economic loss is caused by the sudden ocean oil spill and the industrial wastewater oil pollution, when the surface of seawater is polluted by oil bodies, the oil bodies can rapidly form an airtight oil film on the surface of seawater to influence the reoxygenation of water, fish can become odorous within 24h to seriously influence the living environment of floating organisms in the ocean and destroy the marine ecological balance, therefore, the development of a novel efficient separation material for solving the oil spill and the pollution of organic solvent is an important matter And (5) performing tasks.
However, the existing oil-water separation material mostly faces a series of problems of complex preparation process, low separation flux, incapability of being used in a harsh environment and the like, and the large-scale application of the oil-water separation material is limited.
Disclosure of Invention
The invention aims to provide a preparation method of an oil-water separation material with excellent stability, which is characterized in that zwitterions and a coupling agent are subjected to free radical polymerization reaction to carry out surface chemical grafting modification on cotton cloth, so that a super-hydrophobic/underwater super-oleophobic material with excellent chemical stability is finally obtained, the super-hydrophobic/underwater super-oleophobic material has higher separation flux and good stability under the complex environment of strong acid and strong alkali, and a good foundation is laid for large-scale application of oil-water separation sponges.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of an oil-water separation material with excellent stability comprises the following steps:
the method comprises the following steps: taking a bearing substrate, cleaning and drying;
step two: putting the clean and dry bearing substrate into absolute ethyl alcohol, and drying the substrate after ultrasonic washing for later use;
step three: taking a coupling agent, and dissolving the coupling agent in a mixed solution of deionized water and ammonia water to obtain an intermediate I;
step four: placing the bearing substrate prepared in the step two in the intermediate I prepared in the step three, and stirring and grafting to obtain a substrate to be molded;
step five: and (4) placing the substrate to be molded prepared in the step four in a beaker, adding a displacement reagent and an initiator, and stirring to obtain the super-hydrophilic and underwater super-oleophobic oil-water separation material.
As a preferred technical scheme, the bearing substrate can be cotton cloth, sponge and other base materials used as oil-water separation materials.
As a preferred embodiment, the coupling agent in the third step can be KH570 (gamma-methacryloxypropyltrimethoxysilane).
As a preferable technical scheme, the proportion of the deionized water and the ammonia water in the third step is 10:1 by volume component.
As a preferred technical scheme, the coupling agent, deionized water and ammonia water in the third step are in the following volume component ratio: 3:200:20.
As a preferred technical scheme, in the fourth step, the bearing substrate prepared in the second step is placed in the intermediate I prepared in the third step, the temperature is controlled at 60 ℃, 6H grafting is carried out through stirring, and the substrate to be molded is obtained.
In a preferred embodiment, the displacement agent in step five is SBMA ([2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide), and the initiator is AIBN initiator.
As a preferred technical scheme, the weight ratio of the substitution reagent to the initiator is 30: 1.
As a preferred technical scheme, the reaction condition in the fifth step is stirring 6H at 60 ℃.
Compared with the prior art, the method carries out free radical polymerization reaction on zwitterions and a coupling agent to carry out surface chemical grafting modification on the cotton cloth, and finally obtains the super-hydrophobic/underwater super-oleophobic material with excellent chemical stability.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a graph showing the results of an underwater contact angle test of six kinds of oils such as liquid paraffin according to a method for preparing an oil-water separating material having excellent stability according to the present invention.
FIG. 2 is a graph showing the results of a separation flux test of an oil-water mixture such as peanut oil according to a method for preparing an oil-water separating material having excellent stability according to the present invention.
FIG. 3 is a graph showing the stability test result of the modified cotton cloth in the strong acid environment according to the preparation method of the oil-water separation material with excellent stability.
FIG. 4 is a graph showing the stability test result of the modified cotton cloth in the strong alkali environment according to the preparation method of the oil-water separation material with excellent stability.
FIG. 5 is a flow chart of a method for preparing an oil-water separation material with excellent stability according to the present invention.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the drawings are for illustrative purposes only and are not intended to be limiting, wherein certain elements may be omitted, enlarged or reduced in size, and are not intended to represent the actual dimensions of the product, so as to better illustrate the detailed description of the invention.
Example 1
The method comprises the following steps of carrying out free radical polymerization reaction on zwitterions and a coupling agent, carrying out surface chemical grafting modification on cotton cloth, and then initiating the free radical polymerization reaction on the surface of the cotton cloth to form an oil-water separation material with excellent stability, wherein the method mainly comprises the following two steps:
(1) chemical grafting of cotton surfaces
A4 cm by 4 cm cotton cloth was put in 30ml of an absolute ethanol solution, ultrasonically washed and dried for use, and 0.3 ml of KH570 coupling agent (. gamma. -methacryloxypropyltrimethoxysilane) was dissolved in 20 ml of deionized water, 2 ml of an aqueous ammonia solution, and the cotton cloth was put in the solution and stirred at 60 ℃ for 6 hours to give a KH570 grafted cotton cloth.
(2) Preparation of super-hydrophilic/underwater super-oleophobic cotton cloth
The KH570 grafted cotton cloth was placed in a beaker and stirred, 0.3 g SBMA ([2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide) and 0.01 g AIBN initiator were added to initiate a radical polymerization reaction on the surface of the cotton cloth, and stirred at 60 ℃ for 6 hours to obtain a cotton cloth with super-hydrophilic/underwater super-oleophobic properties.
As shown in fig. 5, the more specific preparation steps are as follows: a preparation method of an oil-water separation material with excellent stability comprises the following steps:
the method comprises the following steps: taking dry and clean cotton cloth, placing the cotton cloth in 30ml of absolute ethyl alcohol solution, and drying the cotton cloth after ultrasonic washing for later use;
step two: dissolving 0.3 ml of KH570 coupling agent in 20 ml of deionized water and 2 ml of ammonia water to obtain a mixed solution;
step three: placing the cotton cloth subjected to ultrasonic washing and drying in the step one into the mixed solution obtained in the step two, and stirring for 6 hours at the temperature of 60 ℃ to obtain KH570 grafted cotton cloth;
step four: placing the KH570 grafted cotton cloth obtained in the third step into a beaker, stirring, adding 0.3 g of SBMA and 0.01 g of AIBN initiator into the beaker, and initiating a free radical polymerization reaction on the surface of the cotton cloth;
step five: stirring at 60 deg.C for 6 hr to obtain cotton cloth with super hydrophilic/super oleophobic property under water.
In this embodiment, the thickness of the cotton cloth in the first step is 0.2cm-0.5 cm.
In this example, the KH570 coupling agent in step two is preferably gamma-methacryloxypropyltrimethoxysilane.
In this embodiment, the volume ratio of the deionized water to the ammonia water in the mixed solution of the deionized water and the ammonia water in the second step is 10:1, and the volume ratio of the KH570 coupling agent to the mixed solution of the deionized water and the ammonia water is 3: 220.
In this example, the mixed solution in the second step and the third step is a mixed solution obtained by dissolving 0.3 ml of gamma-methacryloxypropyltrimethoxysilane sufficiently in a mixed solution of 20 ml of deionized water and 2 ml of ammonia water.
In this example, SBMA in step four is specifically [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide.
In this example, the mass ratio of SBMA to AIBN initiator in step four was 30: 1.
Example 2
In the present invention, the method for testing the underwater contact angle is as follows:
1. opening the contact angle tester and the connected computer: adopt deionized water, drop the water droplet and carry out the test after film surface l min, every sample is got 3 points apart from 5 mm and is measured, and the dropping liquid volume is controlled within 1-5 microliter to the greatest extent, because the dropping liquid is too much, the dropping liquid receives gravity to influence and can change, is not a formal circle or ellipse, if be less than this dropping liquid volume, unless it is very little to test the sample, needs the condition of little dropping liquid, need communicate well with the producer and purchase the micro-level liquid injector.
2. Placing the sample on a sample stage: the brightness of the light source needs to be adjusted according to the actual operation condition, too bright can cause the outline of the liquid drop to be unclear, and too dark can cause the liquid drop to be enlarged or too many black spots around the liquid drop, thereby influencing the accuracy of the test data.
3. And after the software is opened, automatic liquid dropping is carried out, then the sample table is lifted to the position of the liquid receiving baseline, the baseline cannot be identified under special conditions, and an operator needs to manually find the baseline.
4. The measurements were taken at 3 points 5 mm apart for each sample, 6 readings were taken, and the arithmetic mean was taken.
In this example, to confirm the underwater superoleophobic performance of dip-coated cotton, we performed an underwater contact angle test on modified cotton with different oils or organic solvents.
The surface wettability is one of common phenomena in nature and is one of important properties of a solid surface, and the wetting refers to a process of replacing one fluid on the solid surface by another fluid, and when a liquid spreads on the solid surface and a contact surface has a tendency of expanding, the wetting is performed, namely, the adhesion force of the liquid to the solid surface is greater than the cohesion force of the liquid; when the liquid can not spread on the solid surface, the contact surface has the tendency of shrinking into a sphere, namely, the liquid is not wetted, namely, the adhesive force of the liquid to the solid surface is smaller than the cohesive force of the liquid, the wettability of the solid surface is generally measured by a contact angle theta, the tangent of the liquid surface and the tangent of the solid surface are taken at the junction of liquid, solid and gas phases, and the included angle formed by the two tangents in the liquid is the contact angle which is also called the intrinsic contact angle theta of the solid surface; in measuring a contact angle of a solid surface to water, the solid surface has hydrophilicity if 0 ° < θ <90 °, and super-hydrophilicity when θ =0 °; if theta is more than or equal to 90 degrees and less than 150 degrees, the solid surface has hydrophobicity; if theta is larger than or equal to 150 degrees, the solid surface has super-hydrophobic performance, similarly, when the contact angle of the solid surface to oil is measured, if 0 degrees and smaller than theta is less than 90 degrees, the solid surface has lipophilicity, and when theta =0 degrees, the solid surface has super-oleophilic performance; if theta is more than or equal to 90 degrees and less than 150 degrees, the solid surface has certain lipophilicity; if theta is larger than or equal to 150 degrees, the solid surface has super oleophobic performance, so the oleophilic material is a solid material which can be wetted by oil drops, and the surface of the oleophilic hydrophobic oil-water separation material must have high hydrophobic or super hydrophobic property and super oleophilic performance.
In order to confirm the underwater super-oleophobic property of the dip-coated cotton cloth, seven different oils or organic solvents such as liquid paraffin, peanut oil, dimethyl silicone oil, n-hexadecane, dichloromethane, diesel oil, toluene and the like are subjected to an underwater contact angle test on the modified cotton cloth, and the test result is shown in figure 1.
The underwater contact angle of the tested liquid paraffin is about 150 degrees, the underwater contact angle of the tested peanut oil is about 148 degrees, the underwater contact angle of the tested dimethyl silicone oil is about 151 degrees, the underwater contact angle of the tested n-hexadecane is about 153 degrees, the underwater contact angle of the tested dichloromethane is about 149 degrees, the underwater contact angle of the tested diesel oil is about 148 degrees, and the underwater contact angle of the tested diesel oil is about 151 degrees.
As shown in figure 1, the tested underwater contact angles of oil and an organic solvent are both about 150 degrees, wherein the underwater contact angle of n-hexadecane is about 153 degrees, and the contact angle test of the underwater oil and the organic liquid fully shows the underwater super-oleophobic property of the modified cotton cloth, has high hydrophobic or super-hydrophobic property and super-oleophilic property, and lays a theoretical foundation for oil-water separation operation.
Example 3
In this example, oil-water separation tests were performed on different oils or organic solvents through modified cotton cloth.
The modified cotton cloth is subjected to an oil-water separation test, 30ml of deionized water is respectively mixed with 30ml of peanut oil, dichloromethane, n-hexadecane, liquid paraffin, diesel oil, dimethyl silicone oil and toluene, the modified cotton cloth is fixed in a Buchner funnel, and under the action of gravity, the deionized water flows out of the cotton cloth rapidly without oil flowing down, and is completely separated from water only within 9s, which shows that the cotton cloth prepared by the method has high-efficiency oil-water separation capability.
As shown in figure 2, the separation flux of the liquid paraffin is the minimum under the action of gravity, the separation flux is about 17500 Lm-2h-1, the separation flux of the n-hexadecane is the maximum, the separation flux is about 20000 Lm-2h-1, and the separation fluxes of various organic solvents and oil are all more than 16000 Lm-2h-1, which shows that the oil-water separation membrane prepared by the invention has greater application value.
Example 4
The experimental results of the embodiment 1 and the embodiment 2 show that the cotton cloth prepared by the invention has excellent super-hydrophilic/underwater super-oleophobic performance, however, the cotton cloth can be exposed to various harsh environments in actual use, and the stability of the cotton cloth in an acid-base environment is researched.
In this example, the stability of cotton cloth in an acidic environment was first tested to simulate the superhydrophilic/underwater superoleophobic performance of cotton cloth in a strong acid environment.
Firstly, cotton cloth is placed in 6M hydrochloric acid solution to simulate a strong acid environment, the strong acid resistance stability of the cotton cloth is tested by detecting the contact angle of water and the contact angle of oil (n-hexadecane) under water of the cotton cloth soaked for different time, the test result is shown in figure 3, and it can be seen that after the cotton cloth is soaked for different time, the cotton cloth prepared by the method still has super-hydrophilicity in the air and super-lipophobicity under water, the contact angle of the n-hexadecane is stabilized at about 155 degrees, and the cotton cloth still has excellent super-hydrophilicity/super-lipophobicity under water under an acid environment, so that the cotton cloth shows excellent stability to strong acid.
Example 5
In this example, the stability of cotton cloth in alkaline environment was tested to simulate the superhydrophilic/underwater superoleophobic behavior of cotton cloth in a strong alkaline environment.
When the stability of the cotton cloth to a strong alkaline solution is tested, the cotton cloth is placed in a 6M sodium hydroxide strong alkaline solution, the stability of the cotton cloth to the strong alkaline solution is researched through a water contact angle and an underwater oil contact angle of the cotton cloth soaked for different time, and as shown in a figure 4, after the cotton cloth is soaked for more than 24 hours, the cotton cloth is super-hydrophilic in air and still super-oleophobic underwater, the contact angle of oil is maintained at about 152 degrees, the cotton cloth still has excellent super-hydrophilic/underwater super-oleophobic performance in a strong alkaline environment, and the cotton cloth is reflected to have good stability in the strong alkaline environment.
As shown in fig. 1 to 4, through the examples 2 to 5, the underwater contact angle test of different oils or organic solvents on the modified cotton cloth, the oil-water separation test of different oils or organic solvents on the modified cotton cloth, the stability test in an acidic environment, and the stability test in an alkaline environment are respectively performed, and the test results show that the cotton cloth prepared by the method has excellent super-hydrophilic/underwater super-oleophobic properties under different oils or organic solvents, and the cotton cloth still has excellent super-hydrophilic/underwater super-oleophobic properties under strong acidic and strong alkaline environments when the cotton cloth is exposed to various harsh environments in actual use, such as strong acidic and strong alkaline environments, so that the cotton cloth has good stability and excellent chemical stability under the strong alkaline environment.
The method is characterized in that common cotton cloth is modified by a simple chemical grafting method to obtain the cotton cloth with super-hydrophilic/underwater super-oleophobic property, contact angles of underwater oil drops and various organic liquid drops can reach more than 150 degrees, separation fluxes of various organic solvents and oil can reach 16000 Lm-2h-1 only under the action of gravity, and the cotton cloth also has excellent chemical stability and good stability in strong acid and strong alkali solutions, so that the application range of the material is expanded, and a good foundation is laid for large-scale industrialization of oil-water separation sponges.
While there have been shown and described what are at present considered the preferred embodiments of the invention, the fundamental principles and essential features of the invention and advantages thereof, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are included to illustrate the principles of the invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (8)
1. A preparation method of an oil-water separation material with excellent stability is characterized by comprising the following steps:
the method comprises the following steps: taking a bearing substrate, cleaning and drying;
step two: putting the clean and dry bearing substrate into absolute ethyl alcohol, and drying the substrate after ultrasonic washing for later use;
step three: taking KH570 coupling agent (gamma-methacryloxypropyltrimethoxysilane), and dissolving the KH570 coupling agent (gamma-methacryloxypropyltrimethoxysilane) in a mixed solution of deionized water and ammonia water to obtain an intermediate I;
step four: placing the bearing substrate prepared in the step two in the intermediate I prepared in the step three, and stirring and grafting to obtain a substrate to be molded;
step five: and (3) placing the substrate to be molded prepared in the fourth step into a beaker, adding a substitution reagent SBMA ([2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide) and an initiator AIBN, and stirring to obtain the super-hydrophilic and underwater super-oleophobic oil-water separation material.
2. The method for preparing an oil-water separating material having excellent stability as claimed in claim 1, wherein: the bearing substrate can be cotton cloth, sponge and other substrates used as oil-water separation materials.
3. The method for preparing an oil-water separating material having excellent stability as claimed in claim 1, wherein: and the deionized water and the ammonia water in the third step are in a volume component ratio of 10: 1.
4. The method for preparing an oil-water separating material having excellent stability as claimed in claim 1, wherein: the coupling agent, the deionized water and the ammonia water in the third step are in volume component ratio as follows: 3:200:20.
5. The method for preparing an oil-water separating material having excellent stability as claimed in claim 1, wherein: in the fourth step, the bearing substrate prepared in the second step is placed in the intermediate I prepared in the third step, the temperature is controlled to be 60 ℃, and 6H grafting is stirred to obtain the substrate to be molded.
6. The method for preparing an oil-water separating material having excellent stability as claimed in claim 1, wherein: the weight ratio of the metathesis reagent to the initiator was 30: 1.
7. The method for preparing an oil-water separating material having excellent stability as claimed in claim 1, wherein: the reaction conditions in step five were stirring 6H at 60 ℃.
8. The method for producing an oil-water separating material having excellent stability as claimed in any one of claims 1 to 7, wherein an oil-water separating material having excellent stability is produced by any one of the production methods.
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