CN112090116B - Preparation method of oil-water separation membrane - Google Patents
Preparation method of oil-water separation membrane Download PDFInfo
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Abstract
The invention discloses a preparation method of an oil-water separation membrane, belonging to the technical field of oil-water separation, wherein the preparation method of the oil-water separation membrane comprises the following steps: construction of SiO on Cotton fabrics Using solution gel Process2Micro-spherical structure to obtain a loadThe cotton fabric with the silicon dioxide microspheres takes eleostearic acid as a coating material, and natural cotton fabric is modified by a solution gel method. The preparation method provided by the application is simple and easy to operate, the prepared oil-water separation membrane has a good hydrophobic effect, water drops cannot wet the surface of the oil-water separation membrane, but oil drops can smoothly pass through the oil-water separation membrane, so that the cotton fabric base material has a hydrophobic and oleophylic property; the whole preparation process is simple and quick, fluorine is not contained, the cotton fabric base material is low in price and low in preparation cost, the material is environment-friendly, secondary pollution to the environment cannot be caused, and the obtained oil-water separation membrane has the advantages of high separation efficiency, good stability and the like.
Description
Technical Field
The invention belongs to the technical field of oil-water separation, and particularly relates to a preparation method of an oil-water separation membrane.
Background
With the development of human society, environmental deterioration has become a worldwide problem. The increase in the discharge of oily wastewater from the expanding manufacturing industry, as well as the frequent oil leakage accidents, exacerbates the pollution and shortage of water resources. Thus, the current state of affairs has led to a global interest in developing technologies or materials for efficient oil-water separation. Filtration-absorption selective separation techniques are considered to be the most efficient methods due to their high separation efficiency and relatively simple procedures compared to conventional techniques such as skimming, gravity separation and in situ combustion. The development of materials with selective separation properties is key to achieving efficient separation of various oils. Since oil-water separation is essentially an interface problem. Researchers have been working on designing and manufacturing new materials with specific wettabilities to achieve efficient and advantageous oil-water separation. Among them, increasing the surface roughness by nano-micro scale structure and decreasing the surface energy by long chain fluorine containing compounds are the most common strategies for super hydrophobic cotton cloth manufacturing. However, fluorine-containing compounds can have a negative environmental impact due to toxicological consequences. At present, most separation materials are complex in preparation process, and the materials cannot be degraded after being used, so that secondary pollution to the environment is caused, and therefore, the development of an economical, simple, natural and environment-friendly oil-water separation material is a challenge.
Cotton, which is the most widely used material in various domestic and industrial applications, consists of cellulose, has various characteristics such as renewability and biodegradability, and has a large amount of hydroxyl groups on its surface to facilitate surface modification, and thus, cotton cloth is an ideal substrate for separation of oil and water mixtures. The tung oil is a special resource in China, commonly called Chinese wood oil, has very rich yield accounting for about 80 percent of the world yield, and is a renewable resource. The oil film has the performances of firmness, strong adhesion, water resistance, sunlight and atmosphere resistance and the like, and can be widely added into paint, varnish and related substances. The main component of the oil is eleostearic acid. Traditional tung oil based materials show good waterproof property after being coated, for example, the invention patent with the application number of 201610187075.4 discloses a hydrophobic furniture coating and a preparation method thereof, a cross-linking structure is formed by utilizing the direct action of tung oil and perfluoro resin, the waterproof effect of the coating is further improved by the perfluoro resin, but the super-hydrophobic property is not shown. The traditional coating mode enables the acting force between pure eleostearic acid and a cotton cloth base material to be weaker, and the traditional coating mode is not easy to apply to the preparation of oil-water separation materials.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problems to be solved by the invention are as follows: provides a preparation method of an oil-water separation membrane with good oil-water separation effect.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of an oil-water separation membrane comprises the following steps:
step 1: adding absolute ethyl alcohol into a container, then adding a cotton fabric substrate, tetraethoxysilane, distilled water and ammonia water, electrically stirring for 1h, then taking out, washing for 3 times by using the absolute ethyl alcohol, and drying to obtain a cotton fabric loaded with silicon dioxide microspheres;
step 2: and (3) soaking the cotton fabric loaded with the silicon dioxide microspheres obtained in the step (1) in a tung oil acid ethanol solution, and then drying to obtain the oil-water separation membrane.
The invention has the beneficial effects that: the invention utilizes a sol-gel method to modify natural cotton cloth to prepare the cotton fabric loaded with silicon dioxide microspheres, wherein the surface of the cotton fabric is SiO2The microspheres increase the surface roughness of the cotton fabric, eleostearic acid is used as a coating material, and the natural cotton fabric is further modified by a sol-gel method to obtain the natural oil-water separation membrane. Eleostearic acid molecule has long fatty chain, is a wax class material, when further increasing the roughness of cotton fabric, the cotton fabric substrate has hydrophobic oleophylic nature and good hydrophobic effect for the water droplet can not wet oil water separating membrane's surface, but the oil droplet can pass through smoothly, and the contact angle can reach 160, makes the cotton fabric substrate have hydrophobic oleophylic nature and good hydrophobic effect, and the chemical stability of gained oil water separating membrane is good and can manifold cycles use, has avoided the secondary pollution to the environment.
Drawings
FIG. 1 is a schematic view showing the oil-water separation efficiency of the oil-water separation membrane obtained in example 1 according to the embodiment of the present invention;
FIG. 2 is a diagram illustrating the recycling oil-water separation efficiency of the oil-water separation membrane obtained in example 1 according to the present invention;
FIG. 3 is a schematic view showing a change in contact angle of the oil-water separation membrane with ultraviolet light irradiation resistance prepared in example 1 according to the embodiment of the present invention.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
The most key concept of the invention is as follows: using SiO2The oil-water separation membrane with low cost, good separation effect and good chemical stability is prepared by constructing the surface roughness and the hydrophobic effect of eleostearic acid.
The preparation method of the oil-water separation membrane comprises the following steps:
step 1: adding absolute ethyl alcohol into a container, then adding a cotton fabric substrate, tetraethoxysilane, distilled water and ammonia water, electrically stirring for 1h, then taking out, washing for 3 times by using the absolute ethyl alcohol, and drying to obtain a cotton fabric loaded with silicon dioxide microspheres;
And 2, step: and (3) soaking the cotton fabric loaded with the silicon dioxide microspheres obtained in the step (1) in a tung oil acid ethanol solution, and then drying to obtain the oil-water separation membrane.
From the above description, the beneficial effects of the present invention are: the invention utilizes a sol-gel method to modify natural cotton cloth to prepare the cotton fabric loaded with silicon dioxide microspheres, wherein the surface of the cotton fabric is SiO2The microspheres increase the surface roughness of the cotton fabric, eleostearic acid is used as a coating material, and the natural cotton fabric is further modified by a sol-gel method to obtain the natural oil-water separation membrane. Eleostearic acid molecule has long fatty chain, is a wax class material, when further increasing the roughness of cotton fabric, the cotton fabric substrate has hydrophobic oleophylic nature and good hydrophobic effect for the water droplet can not wet oil water separating membrane's surface, but the oil droplet can pass through smoothly, and the contact angle can reach 160, makes the cotton fabric substrate have hydrophobic oleophylic nature and good hydrophobic effect, and the chemical stability of gained oil water separating membrane is good and can manifold cycles use, has avoided the secondary pollution to the environment. According to the invention, the silicon dioxide particles are used for loading the cotton cloth substrate, so that a layer of coarse particle structure is formed on the surface, and the hydrophobic aliphatic hydrocarbon group is enriched on the surface of the film by virtue of the covalent bond formed by the condensation of the carboxyl of eleostearic acid and the silicon dioxide particles rich in hydroxyl, so that the surface energy is reduced, the problem of weak acting force between eleostearic acid and the cotton cloth substrate is solved, and the super-hydrophobic modified cotton cloth can be constructed on the premise of not introducing fluorine or silicon-containing resin, and can be applied to the field of oil-water separation.
Further, the cotton fabric substrate in the step 1 is pretreated, and the pretreatment method comprises the following steps: carrying out ultrasonic treatment on a cotton fabric substrate in acetone, drying, then placing the dried cotton fabric substrate in distilled water for ultrasonic treatment, drying, then placing the cotton fabric substrate in a sodium hydroxide solution for soaking, then taking out the cotton fabric substrate, washing the cotton fabric substrate with distilled water until the washed distilled water is neutral, and then drying.
Further, the ultrasonic treatment time in the pretreatment is 15-20min, the concentration of the sodium hydroxide solution is 0.1mol/L, and the soaking time is 1.5-2.5 h.
As can be seen from the above description, the above pretreatment can remove stains and bio-oil on the surface of the cotton fabric substrate, and the treatment with sodium hydroxide is beneficial to activating and increasing hydroxyl groups of the cotton fabric substrate, so that the cotton fabric substrate can be modified by subsequent steps.
Further, in the step 1, absolute ethyl alcohol is used as a solvent, so that tetraethoxysilane is fully hydrolyzed in the reaction process, and the volume ratio of the absolute ethyl alcohol to the tetraethoxysilane to distilled water to ammonia water in a container is 9:1:1: 1.
Further, the rotation speed of the electric stirring is 400r/min, and the temperature is 50 ℃.
As can be seen from the above description, the proportion of the above components is the optimum proportion, and other proportions may result in insufficient hydrolysis of tetraethoxysilane, too long gelling time, and even failure to form gel or gel particles easily agglomerated and failure to form gel.
Further, in the step 1 and the step 2, the temperature of the drying treatment is 100-120 ℃, and the time is 1-2 h.
As is apparent from the above description, the efficiency of the drying process, i.e., the curing process, can be accelerated by heating in a suitable temperature range.
Further, the cotton fabric base material in the step 1 is cotton cloth.
From the above description, the cotton cloth has wide source, low price, low preparation cost, good mechanical stability and good separation effect.
Further, in the step 2, the solubility of the ethanol eleostearic acid solution is 10mg/mL, 15mg/mL, 20mg/mL, 25mg/mL or 30 mg/mL.
Further, in the step 2, the temperature of the ethanol solution of eleostearic acid is 50 ℃. The attachment of eleostearic acid on the surface of the base material is not facilitated due to too low temperature, and the silicon dioxide particles on the surface of the cotton cloth are easy to damage due to too high temperature, so that the hydrophobic effect is reduced.
Example 1:
a preparation method of an oil-water separation membrane specifically comprises the following steps:
step 1: carrying out ultrasonic treatment on a cotton fabric substrate in acetone for 20min, drying, then placing the cotton fabric substrate in distilled water for ultrasonic treatment for 20min, drying, then placing the cotton fabric substrate in a 0.1mol/L sodium hydroxide solution for soaking for 2h, then taking out, washing with distilled water until the solution is neutral, and then drying to obtain a pretreated cotton fabric substrate;
And 2, step: adding 90mL of absolute ethyl alcohol into a container, then adding a cotton fabric substrate, 10mL of tetraethoxysilane, 10mL of distilled water and 10mL of ammonia water, electrically stirring for 1h, and then taking out, wherein the rotating speed of the electric stirring is 400r/min, and the temperature is 50 ℃; then washing with absolute ethyl alcohol for 3 times, and drying in a drying oven at 120 ℃ for 1h to obtain cotton fabric loaded with silicon dioxide microspheres;
and 3, step 3: soaking the cotton fabric loaded with the silicon dioxide microspheres in 10mg/mL ethanol solution of eleostearic acid at 50 ℃ for 1h, taking out, and drying in a drying oven at 100 ℃ for 2h to obtain the oil-water separation membrane.
Example 2:
a preparation method of an oil-water separation membrane specifically comprises the following steps:
step 1: carrying out ultrasonic treatment on a cotton fabric substrate in acetone for 15min, drying, then placing the cotton fabric substrate in distilled water for ultrasonic treatment for 20min, after drying, placing the cotton fabric substrate in a 0.1mol/L sodium hydroxide solution for soaking for 1.5h, then taking out, washing with distilled water until the solution is neutral, and then drying to obtain a pretreated cotton fabric substrate;
step 2: adding 90mL of absolute ethyl alcohol into a container, then adding a cotton fabric base material, 10mL of ethyl orthosilicate, 10mL of distilled water and 10mL of ammonia water, electrically stirring for 1h, and then taking out, wherein the rotating speed of the electric stirring is 400r/min, and the temperature is 50 ℃; then washing with absolute ethyl alcohol for 3 times, and drying in an oven at 115 ℃ for 1.2h to obtain a cotton fabric loaded with silicon dioxide microspheres;
And 3, step 3: soaking the cotton fabric loaded with the silicon dioxide microspheres in 15mg/mL ethanol solution of eleostearic acid at 50 ℃ for 1h, taking out, and drying in a drying oven at 120 ℃ for 1h to obtain the oil-water separation membrane.
Example 3:
a preparation method of an oil-water separation membrane specifically comprises the following steps:
step 1: carrying out ultrasonic treatment on a cotton fabric substrate in acetone for 18min, drying, then placing the cotton fabric substrate in distilled water for ultrasonic treatment for 15min, after drying, placing the cotton fabric substrate in a 0.1mol/L sodium hydroxide solution for soaking for 2.5h, then taking out, washing with distilled water until the solution is neutral, and then drying to obtain a pretreated cotton fabric substrate;
step 2: adding 90mL of absolute ethyl alcohol into a container, then adding a cotton fabric base material, 10mL of ethyl orthosilicate, 10mL of distilled water and 10mL of ammonia water, electrically stirring for 1h, and then taking out, wherein the rotating speed of the electric stirring is 400r/min, and the temperature is 50 ℃; then washing with absolute ethyl alcohol for 3 times, and drying in a drying oven at 110 ℃ for 1.5h to obtain cotton fabric loaded with silicon dioxide microspheres;
and step 3: soaking the cotton fabric loaded with the silicon dioxide microspheres in 20mg/mL ethanol solution of eleostearic acid at 50 ℃ for 1h, taking out, and drying in a drying oven at 110 ℃ for 1.5h to obtain the oil-water separation membrane.
Example 4:
step 1: carrying out ultrasonic treatment on a cotton fabric substrate in acetone for 15min, drying, then placing the cotton fabric substrate in distilled water for ultrasonic treatment for 20min, after drying, placing the cotton fabric substrate in a 0.1mol/L sodium hydroxide solution for soaking for 2.5h, then taking out, washing with distilled water until the solution is neutral, and then drying to obtain a pretreated cotton fabric substrate;
step 2: adding 90mL of absolute ethyl alcohol into a container, then adding a cotton fabric base material, 25mL of ethyl orthosilicate, 10mL of distilled water and 10mL of ammonia water, electrically stirring for 1h, and then taking out, wherein the rotating speed of the electric stirring is 400r/min, and the temperature is 50 ℃; then washing with absolute ethyl alcohol for 3 times, and drying in a drying oven at 120 ℃ for 1h to obtain cotton fabric loaded with silicon dioxide microspheres;
and step 3: soaking the cotton fabric loaded with the silicon dioxide microspheres in 10mg/mL ethanol solution of eleostearic acid at 50 ℃ for 1h, taking out, and drying in an oven at 115 ℃ for 1.5h to obtain the oil-water separation membrane.
Example 5:
a preparation method of an oil-water separation membrane specifically comprises the following steps:
step 1: carrying out ultrasonic treatment on a cotton fabric substrate in acetone for 20min, drying, then placing the cotton fabric substrate in distilled water for ultrasonic treatment for 15min, after drying, placing the cotton fabric substrate in a 0.1mol/L sodium hydroxide solution for soaking for 2.2h, then taking out, washing with distilled water until the solution is neutral, and then drying to obtain a pretreated cotton fabric substrate;
And 2, step: adding 90mL of absolute ethyl alcohol into a container, then adding a cotton fabric base material, 10mL of ethyl orthosilicate, 10mL of distilled water and 10mL of ammonia water, electrically stirring for 1h, and then taking out, wherein the rotating speed of the electric stirring is 400r/min, and the temperature is 50 ℃; then washing with absolute ethyl alcohol for 3 times, and drying in a drying oven at 100 ℃ for 2 hours to obtain a cotton fabric loaded with silicon dioxide microspheres;
and step 3: soaking the cotton fabric loaded with the silicon dioxide microspheres in 30mg/mL ethanol solution of eleostearic acid at 50 ℃ for 1h, taking out, and drying in a drying oven at 110 ℃ for 1.8h to obtain the oil-water separation membrane.
Experimental example:
1. water contact Angle test
A DSA25 contact angle measuring instrument (KRUSS in Germany) is used for testing, the water contact angle of the oil-water separation membrane can be measured to be about 156 degrees, wherein the contact angle of the super-hydrophobic cotton cloth prepared by 20mg/mL elaeostearic acid ethanol solution can reach 160 degrees at most.
2. Oil-water separation test
Respectively selecting 30g of petroleum ether, n-hexane, cyclohexane, dodecane, gasoline and diesel oil mixed oil, toluene, xylene and dichloromethane mixture and 30g of water to mix to form an oil-water mixture. The oil-water separation membrane prepared in example 3 was sandwiched between two glass tubes to perform oil-water separation, and the quality of oil before and after separation was recorded.
The oil-water separation efficiency is calculated by the following formula:
separation efficiency eta ═ Mt÷M0×100％；
Wherein, M0For the initial oil or water weight before separationAmount, MtIs the weight of oil or water after separation. Oil-water separation is an average value (at least three times) after multiple measurements. FIG. 1 shows the oil-water separation efficiency of the oil-water separation membrane for different types of oil, and it can be seen from FIG. 1 that the separation efficiency of the oil-water separation membrane is 95% or more.
3. Recycle test
The oil-water separation membrane subjected to the oil-water separation test is subjected to an experiment for separating a mixture of n-heptane, xylene and water again, and the separation efficiency is measured, the test result is shown in fig. 2, and it can be seen from fig. 2 that the separation efficiency of the oil-water separation membrane on oil or water is not reduced along with the increase of the cycle number, so that the oil-water separation membrane can be recycled for multiple times.
4. Temperature resistance test
The oil-water separation membrane obtained in example 3 was placed under an ultraviolet lamp having a wavelength of 365nm for ultraviolet irradiation, and a contact angle test was performed every 2 hours until 24 hours. The results are shown in fig. 3, in which the contact angle of the oil-water separation membrane is maintained at 150 ° or more after being irradiated with strong ultraviolet light for different periods of time. Therefore, the oil-water separation membrane has good chemical stability.
Comparative example:
the oil-water separation membranes a to C were obtained by preparing oil-water separation membranes using ethanol solutions of stearic acid, linoleic acid, and lauric acid in equal amounts, respectively, instead of the ethanol solution of eleostearic acid in example 1 under the same conditions, and the contact angles of the oil-water separation membranes a to C were measured, and the results are shown in table 1.
TABLE 1
| Oil-water separation membraneA | Oil-water separation membrane B | Oil-water separation membrane C | |
| Contact angle | 121° | 130° | 125° |
It can be seen that the hydrophobic effect brought about by the eleostearic acid of example 1 is the best.
In conclusion, the invention utilizes the sol-gel method to modify the natural cotton cloth to prepare the cotton fabric loaded with the silicon dioxide microspheres, and the SiO on the surface of the cotton fabric is2The microspheres increase the surface roughness of the cotton fabric, eleostearic acid is used as a coating material, and the natural cotton fabric is further modified by a sol-gel method to obtain the natural oil-water separation membrane. Eleostearic acid molecule has long fatty chain, when further increasing the roughness of cotton fabric, the cotton fabric substrate has hydrophobic oleophylic nature and good hydrophobic effect for the water droplet can not wet oil water separating membrane's surface, but the oil droplet can pass through smoothly, and the contact angle can reach 160, makes the cotton fabric substrate have hydrophobic oleophylic nature and good hydrophobic effect, and the chemical stability of gained oil water separating membrane is good and can manifold cycles use, has avoided the secondary pollution to the environment.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (7)
1. The preparation method of the oil-water separation membrane is characterized by comprising the following steps:
step 1: adding absolute ethyl alcohol into a container, then adding the pretreated cotton fabric base material, tetraethoxysilane, distilled water and ammonia water, electrically stirring for 1h, then taking out, cleaning for 3 times by using the absolute ethyl alcohol, and drying to obtain the cotton fabric loaded with the silicon dioxide microspheres;
step 2: soaking the cotton fabric loaded with the silicon dioxide microspheres obtained in the step 1 in a tung oil acid ethanol solution at 50 ℃, and then drying to obtain an oil-water separation membrane;
the pretreatment method comprises the following steps: carrying out ultrasonic treatment on a cotton fabric substrate in acetone, drying, then placing the dried cotton fabric substrate in distilled water for ultrasonic treatment, drying, then placing the cotton fabric substrate in a sodium hydroxide solution for soaking, then taking out the cotton fabric substrate, washing the cotton fabric substrate with distilled water until the cotton fabric substrate is neutral, and then drying.
2. The method for preparing an oil-water separation membrane according to claim 1, wherein the time of the ultrasonic treatment in the pretreatment is 15 to 20min, the concentration of the sodium hydroxide solution is 0.1mol/L, and the time of the soaking in the pretreatment method is 1.5 to 2.5 h.
3. The method for producing an oil-water separation membrane according to claim 1, wherein in the step 1, the volume ratio of the absolute ethyl alcohol, the tetraethoxysilane, the distilled water and the ammonia water in the container is 9:1:1: 1.
4. The method for producing an oil-water separation membrane according to claim 1, wherein the rotation speed of the electric stirrer in the step 1 is 400r/min, and the temperature is 50 ℃.
5. The method for preparing the oil-water separation membrane as claimed in claim 1, wherein the drying temperature in step 1 and step 2 is 100-120 ℃ for 1-2 h.
6. The method for preparing an oil-water separation membrane according to claim 1, wherein the cotton fabric substrate of step 1 is cotton fabric.
7. The method for producing an oil-water separation membrane according to claim 1, wherein in the step 2, the solubility of the ethanol elaeostearic acid solution is 10mg/mL, 15mg/mL, 20mg/mL, 25mg/mL, or 30 mg/mL.
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| US4297291A (en) * | 1980-06-30 | 1981-10-27 | Bio Systems Research, Inc. | Method of preparing the methyl ester of α-eleostearic acid |
| CN105001389A (en) * | 2015-08-06 | 2015-10-28 | 吉林师范大学 | Polyurethane material and preparation method thereof |
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| US3340213A (en) * | 1964-05-19 | 1967-09-05 | Union Carbide Corp | Coating compositions from monoepoxy alcohols |
| CN104356356B (en) * | 2014-11-28 | 2017-09-22 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of hydrophobic cellulose material |
| CN109235039B (en) * | 2018-08-21 | 2021-05-04 | 福建师范大学泉港石化研究院 | Preparation method of urushiol oil-water separation membrane |
| CN110526337B (en) * | 2019-08-13 | 2022-05-17 | 福建师范大学 | Preparation method of oil-water separation membrane |
| CN111021047B (en) * | 2019-12-03 | 2022-06-07 | 福建师范大学 | Preparation method of natural high-hydrophobicity cotton fabric |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4297291A (en) * | 1980-06-30 | 1981-10-27 | Bio Systems Research, Inc. | Method of preparing the methyl ester of α-eleostearic acid |
| CN105001389A (en) * | 2015-08-06 | 2015-10-28 | 吉林师范大学 | Polyurethane material and preparation method thereof |
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