A method for preparing and applying a cotton fabric-based oil-water separation membrane
By functionalizing cotton fabrics with dopamine, potassium permanganate, silanol, and propylene monomers, a high-performance and low-cost cotton fabric-based oil-water separation membrane was prepared, solving the problems of high water content oil-water separation and ion adsorption in oil and gas extraction, and achieving efficient oil-water separation and lithium ion removal.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-17
- Publication Date
- 2026-04-03
AI Technical Summary
Existing oil-water separation membranes have problems such as unsatisfactory performance, difficulty in obtaining raw materials or high cost in oil and gas extraction, making it difficult to simultaneously meet the needs of oil-water separation with high water content and ion adsorption and desorption.
Cotton fabrics are functionalized using dopamine and potassium permanganate solutions to form a polydopamine layer rich in phenolic hydroxyl and amine groups. Manganese dioxide is formed by potassium permanganate, and propylene-based polymers are formed by combining silanol and propylene monomer solutions, thereby improving oil-water separation efficiency and stability.
The prepared cotton fabric-based oil-water separation membrane exhibits excellent oil-water separation performance, abrasion resistance, and acid and alkali resistance, and has a low cost. It also has the ability to adsorb and remove lithium ions, making it suitable for oil-water separation with high water content.
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Figure CN119838442B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of oil-water separation membrane technology, and in particular to a method for preparing and applying a cotton fabric-based oil-water separation membrane. Background Technology
[0002] In industrial production, especially in the oil and gas extraction industry, oil-water separation is a crucial and highly challenging task. With the continuous extraction of oil and gas resources, a large amount of byproducts containing oil and water mixtures are generated, some of which have a water content exceeding 95%. Efficient and precise separation of these oil-water mixtures is not only crucial for the effective recycling of resources but also involves numerous subsequent environmental treatment processes. Simultaneously, given the numerous industrial applications and environmental governance needs, there is an urgent demand for functional materials capable of effectively adsorbing and removing specific ions. While some existing oil-water separation membranes can achieve oil-water separation to a certain extent, they often suffer from problems such as insufficient performance, difficulty in obtaining raw materials, or high costs, making it difficult to simultaneously meet the practical needs of oil-water separation and ion adsorption / removal for high-water-content byproducts in the oil and gas extraction industry. In the prior art, Chinese invention patent CN116510523A discloses a method for preparing and applying a corrosion-resistant nitrocellulose cotton fabric oil-water separation filter membrane. This separation filter membrane uses cotton fabric as raw material, which is boiled in sodium hypochlorite solution, washed with ethanol and deionized water respectively, and then air-dried at room temperature. It is then impregnated in nitrocellulose solution and air-dried at room temperature. Chinese invention patent CN110526337A discloses a method for preparing an oil-water separation membrane. This method uses a solution-gel method to construct a SiO2 microsphere structure on cotton fabric, obtaining cotton fabric loaded with silica microspheres. Thiophene is then coated onto the surface of the silica microsphere-loaded cotton fabric using a solid-phase coupling method to form polythiophene. Summary of the Invention
[0003] The purpose of this invention is to provide a method for preparing and applying a cotton fabric-based oil-water separation membrane.
[0004] The technical solution adopted by the present invention to achieve the above objectives is as follows:
[0005] A method for preparing a cotton fabric-based oil-water separation membrane includes: placing cotton fabric in a functional solution and performing functionalization treatment to obtain the cotton fabric-based oil-water separation membrane; the functional solution includes at least a dopamine solution and a potassium permanganate solution, wherein the concentration of the dopamine solution is 1-10 g / L and the concentration of the potassium permanganate solution is 0.01-0.1 mol / L;
[0006] Preferably, in the functionalization process, the cotton fabric is first immersed in a dopamine solution, and then immersed in a potassium permanganate solution to obtain an amine-manganese-based cotton fabric, i.e., a cotton fabric-based oil-water separation membrane. When the cotton fabric is treated with the dopamine solution, dopamine undergoes a self-polymerization reaction, forming a polydopamine layer rich in phenolic hydroxyl and amine groups on the surface of the cotton fabric. Subsequently, treatment with the potassium permanganate solution forms manganese dioxide. This functionalization process also transforms the cotton fabric into a cotton fabric-based oil-water separation membrane, which can effectively achieve oil-water separation and possesses good stability.
[0007] Preferably, the mass ratio of cotton fabric used to dopamine solution is 1:50-100; the mass ratio of cotton fabric used to potassium permanganate solution is 1:50-100.
[0008] Preferably, the functional solution further includes a silanol solution, wherein the silanol solution comprises ethanol, tetraethyl orthosilicate, mercaptopropyltriethoxysilane, and 3-aminopropyltrimethoxysilane; the mass ratio of ethanol to tetraethyl orthosilicate is 1-8:1-4, the mass ratio of ethanol to mercaptopropyltriethoxysilane is 1-8:2-5, and the mass ratio of ethanol to 3-aminopropyltrimethoxysilane is 1-8:1-2.
[0009] Preferably, the functional solution further includes a propylene monomer solution, which comprises ethanol, N-phenylacrylamide, acryloyloxytrimethylsilane, and azobisisobutyronitrile; the concentration of N-phenylacrylamide is 0.05-0.5 mol / L, the concentration of acryloyloxytrimethylsilane is 0.05-0.5 mol / L, and the amount of azobisisobutyronitrile is 1-5 wt% relative to the total mass of N-phenylacrylamide and acryloyloxytrimethylsilane. Under the action of azobisisobutyronitrile, N-phenylacrylamide and acryloyloxytrimethylsilane can undergo free radical polymerization, that is, the propylene groups in N-phenylacrylamide and acryloyloxytrimethylsilane polymerize with the mercapto groups on the silica structure of the cotton fabric surface to form a propylene polymer, thereby improving the oil-water separation efficiency of the cotton fabric-based oil-water separation membrane, and maintaining good oil-water separation efficiency even after friction or acid / alkali treatment.
[0010] Preferably, the functionalization process further includes immersing the amine-manganese-based cotton fabric in a silanol solution to obtain a silica-based cotton fabric.
[0011] Preferably, the functionalization process further includes immersing the silica-based cotton fabric in a propylene monomer solution to obtain a functional layer-based cotton fabric, namely, a cotton fabric-based oil-water separation membrane.
[0012] Preferably, the amine-manganese-based cotton fabric is immersed in a silanol solution and stirred at 50-80 °C for 1-5 h; then placed in a sealed container filled with ammonia and reacted at 30-60 °C for 20-60 min.
[0013] Preferably, the silica-based cotton fabric is immersed in a propylene monomer solution and reacted under vacuum at 60-80 °C for 12-24 h.
[0014] Preferably, the cotton fabric is first immersed in a dopamine solution and reacted on a shaker at 100-300 rpm for 12-36 h; then it is immersed in a potassium permanganate solution and reacted at 60-80 ℃ for 6-10 h.
[0015] This invention discloses a cotton fabric-based oil-water separation membrane prepared by the above method.
[0016] This invention discloses the application of the above-mentioned cotton fabric-based oil-water separation membrane in oil and gas extraction.
[0017] This invention discloses a method for preparing a cotton fabric-based oil-water separation membrane, comprising: immersing cotton fabric in a dopamine solution and reacting it in a shaker at 100-300 rpm for 12-36 h, then immersing it in a potassium permanganate solution and reacting it at 60-80 ℃ for 6-10 h, and drying it at 50-70 ℃ to obtain an amine-manganese-based cotton fabric, i.e., a cotton fabric-based oil-water separation membrane.
[0018] Preferably, the concentration of the dopamine solution is 1-10 g / L, and the mass ratio of the amount of cotton fabric used to the mass of the dopamine solution is 1:50-100; the concentration of the potassium permanganate solution is 0.01-0.1 mol / L, and the mass ratio of the amount of cotton fabric used to the mass of the potassium permanganate solution is 1:50-100.
[0019] This invention discloses a method for preparing a cotton fabric-based oil-water separation membrane, comprising two steps: pretreatment of cotton fabric and preparation of the cotton fabric-based oil-water separation membrane.
[0020] Preferably, in the pretreatment of cotton fabrics, the cotton fabrics are immersed in a dopamine solution and reacted on a shaker at a speed of 100-300 rpm for 12-36 h, then immersed in a potassium permanganate solution and reacted at 60-80 ℃ for 6-10 h, and dried at 50-70 ℃ to obtain amine-manganese-based cotton fabrics.
[0021] Preferably, the concentration of the dopamine solution is 1-10 g / L. The mass ratio of the amount of cotton fabric used to the dopamine solution is 1:50-100; the concentration of the potassium permanganate solution is 0.01-0.1 mol / L, and the mass ratio of the amount of cotton fabric used to the potassium permanganate solution is 1:50-100.
[0022] Preferably, in the preparation of the cotton fabric-based oil-water separation membrane, amine-manganese-based cotton fabric is immersed in a silanol solution and stirred at 50-80 °C for 1-5 h. Then, it is placed in a sealed container filled with ammonia and reacted at 30-60 °C for 20-60 min to obtain silica-based cotton fabric. The silica-based cotton fabric is then removed and immersed in a propylene monomer solution, and reacted under vacuum at 60-80 °C for 12-24 h. It is then washed sequentially with ethanol and deionized water, and dried at 60-80 °C to obtain the functional layer cotton fabric, i.e., the cotton fabric-based oil-water separation membrane.
[0023] Preferably, the silanol solution is composed of ethanol, tetraethyl orthosilicate, mercaptopropyltriethoxysilane, and 3-aminopropyltrimethoxysilane, with the mass ratio of ethanol to tetraethyl orthosilicate being 1-8:1-4, the mass ratio of ethanol to mercaptopropyltriethoxysilane being 1-8:2-5, and the mass ratio of ethanol to 3-aminopropyltrimethoxysilane being 1-8:1-2. The mass ratio of the amount of amine-manganese-based cotton fabric used to the silanol solution is 1-10:80-160.
[0024] Preferably, the propylene monomer solution is composed of ethanol, N-phenylacrylamide, acryloyloxytrimethylsilane and azobisisobutyronitrile, wherein the concentration of N-phenylacrylamide is 0.05-0.5 mol / L, the concentration of acryloyloxytrimethylsilane is 0.05-0.5 mol / L, and the amount of azobisisobutyronitrile is 1-5 wt% relative to the total mass of N-phenylacrylamide and acryloyloxytrimethylsilane.
[0025] More preferably, when immersing the amine-manganese-based cotton fabric in a silanol solution, 1,5-glutaric acid monobenzyl ester is added, with a mass ratio of amine-manganese-based cotton fabric to 1,5-glutaric acid monobenzyl ester of 1-5:20-40. The addition of 1,5-glutaric acid monobenzyl ester can graft onto the silica surface and introduce new functional groups. Combined with the effect of forming propylene-based polymers with N-phenylacrylamide and acryloyloxytrimethylsilane, the performance of the cotton fabric-based oil-water separation membrane is further improved.
[0026] This invention functionalizes cotton fabrics by first immersing them sequentially in a dopamine solution and a potassium permanganate solution, then drying them. Next, the fabrics are immersed in a silanol solution and reacted in a sealed container filled with ammonia gas. Finally, they are submerged in a propylene monomer solution and reacted under vacuum. After washing and drying, a cotton fabric-based oil-water separation membrane is obtained. This results in the following advantages: excellent oil-water separation performance, abrasion resistance, acid and alkali resistance, widely available and low-cost raw materials, and the ability to adsorb and remove lithium ions simultaneously during oil-water separation. Therefore, the purpose of this invention is to provide a method for preparing a high-performance, readily available, and low-cost cotton fabric-based oil-water separation membrane, solving the problem of oil-water separation of by-products in oil and gas extraction, especially by-products with a water content greater than 95%. Attached Figure Description
[0027] Figure 1 The graph shows the test results of the dynamic adsorption capacity and adsorption efficiency of the cotton fabric-based oil-water separation membrane in Example 1.
[0028] Figure 2 The graph shows the test results of the Li(Ⅰ) desorption rate of the cotton fabric-based oil-water separation membrane in Example 1.
[0029] Figure 3 The figure shows the results of the abrasion resistance stability test of the cotton fabric-based oil-water separation membrane.
[0030] Figure 4 The figure shows the acid and alkali resistance stability test results of the cotton fabric-based oil-water separation membrane. Detailed Implementation
[0031] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0032] The concepts involved in this application will first be described with reference to the accompanying drawings. It should be noted that the following descriptions of various concepts are only for the purpose of making the content of this application easier to understand and do not constitute a limitation on the scope of protection of this application; furthermore, the embodiments and features in the embodiments of this application can be combined with each other unless otherwise specified. This application will now be described in detail with reference to the accompanying drawings and embodiments.
[0033] Example 1
[0034] Five g of cotton fabric was immersed in 100 g of a 2 g / L dopamine solution and reacted on a shaker at 150 rpm for 24 h. Then it was immersed in 100 g of a 0.05 mol / L potassium permanganate solution and reacted at 80 ℃ for 8 h. After drying at 60 ℃, amine-manganese-based cotton fabric was obtained, which is a cotton fabric-based oil-water separation membrane.
[0035] Example 2
[0036] Five g of cotton fabric was immersed in 100 g of a 2 g / L dopamine solution and reacted on a shaker at 150 rpm for 24 h. Then, it was immersed in 100 g of a 0.05 mol / L potassium permanganate solution and reacted at 80 ℃ for 8 h. Finally, it was dried at 60 ℃ to obtain amine-manganese-based cotton fabric.
[0037] Five g of amine-manganese-based cotton fabric was immersed in 100 g of silanol solution and stirred at 80 °C for 2 h. Then, it was placed in a sealed container filled with ammonia and reacted at 50 °C for 30 min to obtain silica-based cotton fabric. The silica-based cotton fabric was then removed and immersed in a propylene monomer solution, reacted under vacuum at 70 °C for 18 h, and then washed sequentially with ethanol and deionized water, and dried at 80 °C to obtain the functional layer cotton fabric, i.e., the cotton fabric-based oil-water separation membrane. The silanol solution consisted of ethanol, tetraethyl orthosilicate, mercaptopropyltriethoxysilane, and 3-aminopropyltrimethoxysilane. The mass ratio of ethanol to tetraethyl orthosilicate was 5:3, the mass ratio of ethanol to mercaptopropyltriethoxysilane was 5:2, and the mass ratio of ethanol to 3-aminopropyltrimethoxysilane was 5:1. The propylene monomer solution consists of ethanol, N-phenylacrylamide, acryloyloxytrimethylsilane, and azobisisobutyronitrile. The concentration of N-phenylacrylamide is 0.1 mol / L, the concentration of acryloyloxytrimethylsilane is 0.1 mol / L, and the amount of azobisisobutyronitrile is relative to the total mass of N-phenylacrylamide and acryloyloxytrimethylsilane, which is 2 wt%.
[0038] Example 3
[0039] The difference between this embodiment and Example 2 is that the concentration of N-phenylacrylamide in the propylene monomer solution is 0.2 mol / L, the concentration of acryloyloxytrimethylsilane is 0.2 mol / L, and the rest is the same as in Example 2.
[0040] Example 4
[0041] Five g of cotton fabric was immersed in 100 g of a 2 g / L dopamine solution and reacted on a shaker at 150 rpm for 24 h. Then, it was immersed in 100 g of a 0.05 mol / L potassium permanganate solution and reacted at 80 ℃ for 8 h. Finally, it was dried at 60 ℃ to obtain amine-manganese-based cotton fabric.
[0042] Five g of manganese-based amine-based cotton fabric was immersed in 100 g of silanol solution, and 0.25 g of 1,5-glutaric acid monobenzyl ester was added. The mixture was stirred at 80 °C for 2 h, and then placed in a sealed container filled with ammonia gas. The reaction was carried out at 50 °C for 30 min to obtain silica-based cotton fabric. The silica-based cotton fabric was then removed and immersed in a propylene monomer solution, and reacted under vacuum at 70 °C for 18 h. It was then washed successively with ethanol and deionized water, and dried at 80 °C to obtain a functional layer cotton fabric, i.e., a cotton fabric-based oil-water separation membrane. The silanol solution consisted of ethanol, tetraethyl orthosilicate, mercaptopropyltriethoxysilane, and 3-aminopropyltrimethoxysilane. The mass ratio of ethanol to tetraethyl orthosilicate was 5:3, the mass ratio of ethanol to mercaptopropyltriethoxysilane was 5:2, and the mass ratio of ethanol to 3-aminopropyltrimethoxysilane was 5:1. The propylene monomer solution consists of ethanol, N-phenylacrylamide, acryloyloxytrimethylsilane, and azobisisobutyronitrile. The concentration of N-phenylacrylamide is 0.1 mol / L, the concentration of acryloyloxytrimethylsilane is 0.1 mol / L, and the amount of azobisisobutyronitrile is relative to the total mass of N-phenylacrylamide and acryloyloxytrimethylsilane, which is 2 wt%.
[0043] Example 5
[0044] The difference between this embodiment and embodiment 4 is that when the amine manganese-based cotton fabric is immersed in the silanol solution, the weight of 1,5-glutaric acid monobenzyl ester added is 0.125 g, and the rest is the same as in embodiment 4.
[0045] Comparative Example 1
[0046] The difference between this comparative example and Example 2 is that the propylene monomer solution does not contain acryloyloxytrimethylsilane; otherwise, it is the same as Example 2.
[0047] Comparative Example 2
[0048] The difference between this comparative example and Example 2 is that the propylene monomer solution does not contain N-phenylacrylamide; otherwise, it is the same as Example 2.
[0049] Comparative Example 3
[0050] The difference between this comparative example and Example 4 is that the propylene monomer solution does not contain acryloyloxytrimethylsilane and N-phenylacryloyl, otherwise it is the same as Example 4.
[0051] Li(I) dynamic adsorption capacity and adsorption efficiency test
[0052] Effect of the number of separations on the dynamic adsorption capacity and adsorption efficiency of Li(I): At 25 °C, a 35 mg / L lithium chloride solution was mixed with n-hexane at a volume ratio of 7:3. Using the cotton fabric-based oil-water separation membrane from Example 1 as the separation membrane, the mixture was poured into a container on the membrane for filtration. A separate beaker below the membrane collected the liquid passing through. A total of ten oil-water separation experiments were conducted. The dynamic adsorption capacity was calculated as: Q = (C0 - C) / m, where C0 is the initial content of Li(I), C is the content of Li(I) in the cotton fabric-based oil-water separation membrane after each oil-water separation experiment or after reaching a certain temperature and time, and m is the mass of the cotton fabric-based oil-water separation membrane. The adsorption efficiency was calculated as: E = Q / Q0 × 100%, where Q is the adsorption capacity of Li(I) in the cotton fabric-based oil-water separation membrane after each oil-water separation experiment, and Q0 is the initial content of Li(I).
[0053] Effects of separation time and temperature on Li(I) adsorption: 100 mL of 100 mg / L lithium chloride solution and 0.4 g of cotton fabric-based oil-water separation membrane from Example 1 were placed in a beaker, and the adsorption amount was observed and recorded over time or at temperature in a shaker.
[0054] The results of Li(I) dynamic adsorption and adsorption efficiency tests are as follows: Figure 1 As shown, Figure 1 (a) shows the effect of the number of separations on the amount of adsorption. Figure 1 (b) shows the effect of the number of separations on the adsorption efficiency. Figure 1 (c) shows the effect of separation time on the adsorption amount. Figure 1 (d) shows the effect of separation temperature on the amount of adsorption. It can be seen that during the oil-water separation process, the adsorption capacity of the cotton fabric-based oil-water separation membrane in Example 1 for Li(I) gradually increased. After completing the tenth oil-water separation experiment, the cumulative adsorption capacity reached 10.25 mg / g, indicating that the cotton fabric-based oil-water separation membrane in Example 1 has good Li(I) adsorption capacity. Conversely, the adsorption efficiency of Li(I) gradually decreased with the increase of separation times, from the initial 82% to 38.9%, a reduction of about 43.1%. This indicates that after repeated use of the cotton fabric-based oil-water separation membrane, the Li(I) adsorption efficiency of the membrane will decrease. It can also be seen that as time goes by, the adsorption capacity of the cotton fabric-based oil-water separation membrane in Example 1 for Li(I) shows an upward trend, and the adsorption capacity basically stabilizes at 60 minutes, reaching an adsorption equilibrium state, at which time the adsorption equilibrium capacity is 7.85 mg / g. It can also be seen that as the temperature gradually increases, the initial adsorption capacity of Li(I) increases, but after the temperature exceeds 45 °C, the adsorption capacity begins to show a downward trend, from the previous 8.2 mg / g to 5.46 mg / g. The decrease in oil-water separation membrane was 33.41% (mg / g), indicating that it is more suitable for use when the ambient temperature is below 45 ℃.
[0055] Li(Ⅰ) desorption rate test
[0056] The cotton fabric-based oil-water separator from Example 1, containing 10.2 mg / g Li(Ⅰ), was rinsed with a 0.04 mol / L sulfuric acid solution at a rate of 20 mL / min for 120 s. The Li(Ⅰ) desorption rate was calculated using the formula: Ae = (C0 - C t ) / C0×100%, where C0 is the initial Li(Ⅰ) content in the cotton fabric-based oil-water separation membrane, C t The content of residual Li(Ⅰ) in the cotton fabric-based oil-water separation membrane is given by the washing time.
[0057] The Li(Ⅰ) desorption rate test results are as follows: Figure 2 As shown, it can be seen that during the continuous rinsing for 120 s, the desorption rate of Li(Ⅰ) gradually increases, reaching 95% at 120 s. This indicates that the Li(Ⅰ) adsorbed by the cotton fabric-based oil-water separation membrane can be eluted by the sulfuric acid solution, and the desorption time is relatively short, which is beneficial to the recovery of Li(Ⅰ).
[0058] abrasion resistance stability test
[0059] Abrasion resistance tests were conducted to compare the oil-water separation efficiency before and after the test, evaluating the abrasion resistance stability of the cotton fabric-based oil-water separation membrane. The abrasion resistance test involved placing the cotton fabric-based oil-water separation membrane and a 50 g weight sequentially on 500-grit sandpaper, dragging the sandpaper forward approximately 20 cm in one direction, and repeating this cycle three times. The oil-water separation efficiency was modeled using a mixture of dichloromethane and water, with water comprising 95 wt%. Dichloromethane was stained with Sudan Red, and water with methylene blue. The cotton fabric-based oil-water separation membrane was used as the separation membrane. The oil-water mixture was poured into a container on the membrane for filtration, while a separate beaker below the membrane collected the liquid passing through. The mass of oil before and after separation was recorded, and the separation efficiency was calculated. The formula for calculating the separation efficiency is: R = (m0 / m1) × 100%, where m0 is the mass of oil after separation, and m1 is the mass of oil before separation. The formula for calculating the performance retention rate is: P=R2 / R1×100%, where R1 is the oil-water separation efficiency of the cotton fabric-based oil-water separation membrane before the abrasion resistance test, and R2 is the oil-water separation efficiency of the cotton fabric-based oil-water separation membrane after the abrasion resistance test.
[0060] The results of the abrasion resistance stability test are as follows: Figure 3As shown, the cotton fabric-based oil-water separation membranes of Examples 1 and 2 maintain good performance after the abrasion resistance test, with a high performance retention rate, indicating high abrasion resistance stability. It can also be seen that the performance retention rates of the cotton fabric-based oil-water separation membranes of Examples 2 and 3 are higher than that of Example 1. This indicates that the propylene groups introduced from N-phenylacrylamide and acryloyloxytrimethylsilane can undergo a polymerization reaction with the thiol groups on the silica structure of the cotton fabric surface to form propylene polymers, enhancing abrasion resistance stability and improving the performance retention rate of the cotton fabric-based oil-water separation membrane. Furthermore, it can be seen that the performance retention rate of the cotton fabric-based oil-water separation membrane of Example 2 is higher than that of Example 3. This indicates that the amount of N-phenylacrylamide and acryloyloxytrimethylsilane used in the propylene monomer solution does not necessarily lead to better performance retention. Finally, it can be seen that the performance retention rates of the cotton fabric-based oil-water separation membranes of Examples 4 and 5 are higher than that of Example 2. This indicates that the addition of 1,5-glutaric acid monobenzyl ester during immersion in the silanol solution can modify the silica structure on the cotton fabric surface, increasing the abrasion resistance of the cotton fabric. The surface roughness of the fabric-based oil-water separation membrane improves the performance retention rate. It can also be seen that the performance retention rate of the cotton fabric-based oil-water separation membrane in Example 4 is higher than that in Example 5, indicating that adding an appropriate amount of 1,5-glutaric acid monobenzyl ester can improve the performance retention rate of the cotton fabric-based oil-water separation membrane. Furthermore, it can be seen that the performance retention rate of the cotton fabric-based oil-water separation membrane in Example 2 is higher than that in Comparative Examples 1 and 2, indicating that introducing a propylene-based polymer formed by the polymerization of N-phenylacrylamide and acryloyloxytrimethylsilane with thiol groups on the surface silica structure of the cotton fabric-based oil-water separation membrane results in a higher performance retention rate than introducing a single substance to form a propylene-based polymer on the surface. It can also be seen that the performance retention rate of the cotton fabric-based oil-water separation membrane in Example 4 is higher than that in Comparative Example 3, indicating that the effect of introducing 1,5-glutaric acid monobenzyl ester to modify the silica surface on improving the performance retention rate is lower than the effect of introducing a combination of N-phenylacrylamide, acryloyloxytrimethylsilane, and 1,5-glutaric acid monobenzyl ester.
[0061] Acid and alkali stability test
[0062] Acid and alkali resistance tests were conducted to compare the oil-water separation efficiency before and after the tests, evaluating the acid and alkali resistance stability of the cotton fabric-based oil-water separation membrane. The cotton fabric-based oil-water separation membrane of the example was sequentially immersed in hydrochloric acid solution (pH 3) and sodium hydroxide solution (pH 11) for 12 hours. The performance retention rate was calculated using the formula: P = R2 / R1 × 100%, where R1 is the oil-water separation efficiency of the cotton fabric-based oil-water separation membrane before the acid and alkali resistance test, and R2 is the oil-water separation efficiency of the cotton fabric-based oil-water separation membrane after the acid and alkali resistance test.
[0063] The results of the acid and alkali stability test are as follows: Figure 4As shown in the figures, the cotton fabric-based oil-water separation membranes of Examples 1 and 2 maintained good performance after acid and alkali resistance tests, exhibiting a high performance retention rate, indicating good acid and alkali resistance stability. Furthermore, the performance retention rates of the cotton fabric-based oil-water separation membranes of Examples 2 and 3 were higher than that of Example 1. This indicates that the propylene groups introduced from N-phenylacrylamide and acryloyloxytrimethylsilane can polymerize with the thiol groups on the silica structure of the cotton fabric surface, forming propylene polymers and improving the performance retention rate of the cotton fabric-based oil-water separation membrane. It is also evident that the performance retention rate of the cotton fabric-based oil-water separation membrane of Example 2 was higher than that of Example 3, suggesting that the amount of N-phenylacrylamide and acryloyloxytrimethylsilane used in the propylene monomer solution does not necessarily lead to higher performance retention. Finally, the performance retention rates of the cotton fabric-based oil-water separation membranes of Examples 4 and 5 were higher than that of Example 2, indicating that the grafting of 1,5-glutaric acid monobenzyl ester onto the silica surface, along with the introduction of new groups and the propylene polymers formed by N-phenylacrylamide and acryloyloxytrimethylsilane, combined with the effect of... Modifying the silica structure on the surface improves the performance retention rate of the cotton fabric-based oil-water separation membrane. It can also be seen that the performance retention rate of the cotton fabric-based oil-water separation membrane in Example 4 is higher than that in Example 5, indicating that adding an appropriate amount of 1,5-glutaric acid monobenzyl ester can improve the performance retention rate of the cotton fabric-based oil-water separation membrane. Furthermore, it can be seen that the performance retention rate of the cotton fabric-based oil-water separation membrane in Example 2 is higher than that in Comparative Examples 1 and 2, indicating that introducing a propylene-based polymer formed by the polymerization of N-phenylacrylamide and acryloyloxytrimethylsilane with thiol groups on the surface silica structure of the cotton fabric-based oil-water separation membrane improves the performance retention rate more than introducing a single substance to form a propylene-based polymer on the surface. It can also be seen that the separation efficiency of the cotton fabric-based oil-water separation membrane in Example 4 is higher than that in Comparative Example 3, indicating that simply introducing 1,5-glutaric acid monobenzyl ester to modify the silica surface of the cotton fabric-based oil-water separation membrane has a lower effect on improving the performance retention rate than introducing a combination of N-phenylacrylamide, acryloyloxytrimethylsilane, and 1,5-glutaric acid monobenzyl ester.
[0064] The embodiments and / or implementation methods described above are merely preferred embodiments and / or implementation methods for implementing the technology of the present invention, and are not intended to limit the implementation methods of the technology of the present invention in any way. Any person skilled in the art can make some modifications or alterations to other equivalent embodiments without departing from the scope of the technical means disclosed in the content of the present invention, but they should still be regarded as the technology or embodiments that are substantially the same as the present invention.
[0065] This document uses specific examples to illustrate the principles and implementation methods of this application. The descriptions of the above embodiments are only for the purpose of helping to understand the methods and core ideas of this application. The above descriptions are only preferred embodiments of this application. It should be noted that due to the limitations of written expression, while there are objectively infinite specific structures, those skilled in the art can make several improvements, modifications, or changes without departing from the principles of this application, and can also combine the above technical features in an appropriate manner. These improvements, modifications, changes, or combinations, or the direct application of the inventive concept and technical solution to other situations without modification, should all be considered within the scope of protection of this application.
Claims
1. A method for preparing a cotton fabric-based oil-water separation membrane, comprising: A cotton fabric-based oil-water separation membrane was prepared by functionalizing cotton fabric in a functional solution. The functional solution includes dopamine solution, potassium permanganate solution, silanol solution and propylene monomer solution, wherein the concentration of dopamine solution is 1-10 g / L and the concentration of potassium permanganate solution is 0.01-0.1 mol / L; The silanol solution comprises ethanol, tetraethyl orthosilicate, mercaptopropyltriethoxysilane, and 3-aminopropyltrimethoxysilane; the mass ratio of ethanol to tetraethyl orthosilicate is 1-8:1-4, the mass ratio of ethanol to mercaptopropyltriethoxysilane is 1-8:2-5, and the mass ratio of ethanol to 3-aminopropyltrimethoxysilane is 1-8:1-2. The propylene monomer solution comprises ethanol, N-phenylacrylamide, acryloyloxytrimethylsilane, and azobisisobutyronitrile; the concentration of N-phenylacrylamide is 0.05-0.5 mol / L, the concentration of acryloyloxytrimethylsilane is 0.05-0.5 mol / L, and the amount of azobisisobutyronitrile is 1-5 wt% relative to the total mass of N-phenylacrylamide and acryloyloxytrimethylsilane. In the functionalization process, the cotton fabric is first immersed in a dopamine solution and then in a potassium permanganate solution to obtain an amine-manganese-based cotton fabric. The functionalization process also includes immersing the amine-manganese-based cotton fabric in a silanol solution to obtain a silica-based cotton fabric. The functionalization process also includes immersing silica-based cotton fabric in a propylene monomer solution to obtain a functional layer-based cotton fabric, namely a cotton fabric-based oil-water separation membrane.
2. The method for preparing a cotton fabric-based oil-water separation membrane according to claim 1, characterized in that: The mass ratio of cotton fabric used to dopamine solution is 1:50-100; the mass ratio of cotton fabric used to potassium permanganate solution is 1:50-100.
3. The method for preparing a cotton fabric-based oil-water separation membrane according to claim 1, characterized in that: The amine-manganese-based cotton fabric is immersed in a silanol solution and stirred at 50-80 °C for 1-5 h; then placed in a sealed container filled with ammonia and reacted at 30-60 °C for 20-60 min.
4. The method for preparing a cotton fabric-based oil-water separation membrane according to claim 1, characterized in that: The silica-based cotton fabric is immersed in a propylene monomer solution and reacted under vacuum conditions at 60-80 °C for 12-24 h.
5. The cotton fabric-based oil-water separation membrane prepared by any one of the methods described in claims 1-4.
6. The application of the cotton fabric-based oil-water separation membrane according to claim 5 in oil and gas extraction.
Citation Information
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