CN110655676B - Preparation method of super-hydrophobic sponge with emulsion separation function - Google Patents
Preparation method of super-hydrophobic sponge with emulsion separation function Download PDFInfo
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Abstract
The invention discloses a preparation method of an emulsion separation super-hydrophobic sponge. Soaking commercial polymer sponge into prepared polyacrylic acid, chitosan solution and suspension containing magnesium hydroxide in sequence in a dip-coating mode, and washing and drying to obtain sponge with a micro-nano structure on the surface; and then, treating the obtained sponge by using a surfactant with low surface energy, and cleaning and drying to obtain the super-hydrophobic sponge capable of realizing emulsion separation. The emulsion separation super-hydrophobic sponge can be used for separating oil-in-water type oil-water mixed emulsion with stable surfactant, has the advantages of high separation efficiency, high repeatable utilization rate, large adsorption capacity, high flux and the like, and is simple in process, mild in condition, green, environment-friendly, low in price, convenient and fast, short in preparation period and easy to realize large-scale production and application.
Description
Technical Field
The invention belongs to the technical field of oil-water emulsion separation, and relates to a method for preparing super-hydrophobic sponge for emulsion separation by modifying polymer sponge by utilizing nanotechnology and surface modification technology.
Background
Oily wastewater is used as an important pollution source worldwide, and has serious negative effects on various aspects such as ecological environment, social economy, body health and the like. The generation of the oily wastewater pollution mainly originates from the direct discharge of the oily wastewater in the industrial fields of petrochemical industry, textile dyeing and finishing, metal smelting, food processing and the like, and the oil leakage in the processes of exploration, development, transportation and the like of marine petroleum. The development of materials and processes with high-efficiency separation capability on the oily wastewater has wide practical application value. At present, a large number of effective methods are reported for separating the layered oil-water mixture, and various efficient materials are developed for separating the layered oil-water mixture. The separation of oil and water emulsion as a milky oil and water mixture is more difficult than the separation of a layered oil and water mixture, and at least comprises two processes of demulsification and oil-water separation. In particular industrial practice, the oil-water emulsion is more stable and uniform and difficult to separate simply due to the complex composition and the surfactant, which is the difficult point of oil-water emulsion separation. The common super-hydrophobic super-oleophilic surface is widely applied to the field of oil-water separation because of selective oil absorption and complete water non-absorption, but most super-hydrophobic super-oleophilic materials can only be used for separating simple layered oil-water mixtures. Therefore, the search for a separation material that can achieve effective demulsification of a stable, homogeneous emulsion containing a surfactant and simultaneously perform oil-water separation has become a worldwide problem that is still in need of solution and is full of challenges.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a method for separating an oil-water emulsion.
The invention adopts the composite polymer sponge material with super-hydrophobic property to separate oil and water emulsion; the polymer sponge is prepared by loading nano layered particles, dip-coating the nano layered particles in a surfactant with low surface energy, and drying the nano layered particles in an oven, has super-hydrophobic and super-oleophilic properties in air, and can realize the rapid separation of oil-water emulsion under the action of gravity or stirring.
The technical scheme adopted by the invention comprises the following steps:
1) soaking the polymer sponge into a polyacrylic acid-containing aqueous solution, chitosan-containing dispersion and suspension containing nano magnesium hydroxide particles, washing and drying to obtain a sponge with a micro-nano structure;
2) and (3) treating the dried sponge with the micro-nano structure by adopting a surfactant with low surface energy, and drying to obtain the super-hydrophobic sponge for realizing emulsion separation.
Furthermore, the polymer sponge is three-dimensional porous melamine sponge or polyurethane sponge with the characteristics of low cost, light weight, small pore diameter, high adsorption capacity, good elasticity and the like.
Further, the polyacrylic acid solution has a pH of 1 and a content of 0.1 wt%, and is obtained after stirring at a constant speed for 1 hour.
Further, the polyacrylic acid solution with pH of 1 is obtained by dropping a certain volume of dilute hydrochloric acid with a content of 1M while stirring.
Further, the chitosan solution had a pH of 5 and a content of 0.5 wt%, and was uniformly stirred for 12 hours.
Further, the chitosan solution with pH of 5 is obtained by dropping a certain volume of dilute hydrochloric acid with a content of 1M during stirring.
Further, the magnesium hydroxide suspension has a pH of 10 and a content of 0.05-0.5 wt%, and is prepared by stirring at a constant speed for 12 hours.
Further, the magnesium hydroxide suspension having a pH of 10 was obtained by dropping a predetermined volume of 0.2M sodium hydroxide during stirring.
Furthermore, the nanoscale lamellar magnesium hydroxide particles are prepared by firstly adding a certain amount of surfactant into a sodium hydroxide aqueous solution through a reverse precipitation method; then, the magnesium chloride solution was slowly added dropwise to the above sodium hydroxide aqueous solution containing a surfactant. Wherein the molar ratio of the sodium hydroxide to the magnesium chloride is 1: 2. After the reaction is finished, continuously aging the mother liquor for 3 hours under the stirring state; aging, washing the product with deionized water for many times, drying at 120 deg.C for 3 hr, grinding, and sieving.
Furthermore, the surfactant is Cetyl Trimethyl Ammonium Bromide (CTAB), Sodium Dodecyl Benzene Sulfonate (SDBS) and the like, and the addition amount of the surfactant is 2-4% of the theoretical yield of the magnesium hydroxide.
Further, the low surface energy surfactant is a stearic acid solution with the concentration of 0.005-0.1M.
Further, the method for treating the sponge with the micro-nano structure by using the low-surface-energy substance solution comprises the steps of directly soaking the sponge in a stearic acid-ethanol solution for 2-8 hours, taking out and drying.
Further, the emulsion separation super-hydrophobic sponge can be used for separation of oil-in-water oil-water mixed emulsion stabilized by containing surfactant.
Further, the oil-in-water type oil-water mixed emulsion containing the stable surfactant is prepared by stirring a mixture of the surfactant, oil and water under ultrasonic or high rotating speed.
Further, the surfactant is any one of Cetyl Trimethyl Ammonium Bromide (CTAB), Sodium Dodecyl Sulfate (SDS), Tween 80(Tween-80) and the like; the oil is any one of n-heptane, n-hexane, dodecane, toluene, chlorobenzene or n-octane; the content of the surfactant in the emulsion is 0.01-1 g/L; the volume ratio of oil to water in the emulsion is 1/100-1/9.
The emulsion separation super-hydrophobic sponge prepared by the method has the advantages of no toxicity, no harm, economy, low cost, environmental protection, simplicity, easy obtaining, large-scale preparation realization and the like.
The emulsion separation super-hydrophobic sponge prepared by the method provided by the invention has the advantages of simple and quick process, cheap and easily obtained raw materials, long-acting energy-saving method because the preparation is basically carried out under normal temperature conditions except drying (or normal temperature drying), wide application range and easy realization of large-scale industrial production, and can be used for treating various substrate materials.
According to the invention, after the synthesized nanoparticles are loaded on the surface of the sponge, the separation performance of the sponge on an oil-water mixture can be regulated and improved, and particularly the separation performance of the sponge on an oil-in-water oil-water mixed emulsion containing stable surfactants is improved.
The emulsion separation super-hydrophobic sponge prepared by the invention has the advantages of high separation efficiency, large flux, good reusability and the like.
Drawings
FIG. 1 is a scanning electron micrograph of a superhydrophobic sponge having an emulsion separation function according to example 1 of the present invention.
FIG. 2 is a photograph showing a contact angle of 4.0. mu.L of deionized water on a superhydrophobic sponge having an emulsion separation function according to example 1 of the present invention.
FIG. 3 is a comparative view showing the separation of the oil-in-water type emulsion containing sodium lauryl sulfate by the super hydrophobic sponge having the emulsion separating function in example 1 of the present invention.
FIG. 4 is a comparative graph of the superhydrophobic sponge having an emulsion separation function according to example 2 of the present invention before and after separation of an oil-in-water emulsion containing cetyltrimethylammonium bromide.
Detailed Description
The present invention will be further described, but not limited to, by the following specific embodiments in conjunction with the accompanying drawings.
It should be noted that the embodiment is only used for further illustration of the present invention, and should not be construed as limiting the scope of the present invention, and the modification and modification made by those skilled in the art based on the above disclosure are also considered to fall within the scope of the present invention. It is emphasized that the dimensions of the substrate in the embodiments described herein are merely provided to illustrate the invention in detail and are not intended to limit the invention.
The invention provides a preparation method and application of an emulsion separation super-hydrophobic sponge, wherein the method comprises the following process steps and conditions:
example 1
320mL of 0.6M aqueous sodium hydroxide solution were prepared and added theoreticallyPreparing Sodium Dodecyl Benzene Sulfonate (SDBS) with the mass of 3 percent of the magnesium hydroxide, and stirring for 10 min; then, 80mL of 1.2M MgCl chloride was prepared2The solution was slowly added dropwise to the above aqueous sodium hydroxide solution containing SDBS. After the reaction is finished, continuously aging the mother liquor for 3 hours under the stirring state; after aging, the product was washed with deionized water several times, dried in an oven at 120 ℃ for 3 hours, ground, and sieved to obtain SDBS-containing nano-sized magnesium hydroxide particles (S-MH).
Firstly, soaking commercial melamine sponge into 100mL of polyacrylic acid aqueous solution with the pH value of 1 and the content of 0.1 wt%, wringing out the commercial melamine sponge, then soaking the commercial melamine sponge into 100mL of chitosan dispersion with the pH value of 5 and the content of 0.5 wt%, wringing out the commercial melamine sponge, soaking the commercial melamine sponge into ultrapure water, then soaking the commercial melamine sponge into 100mL of magnesium hydroxide suspension with the pH value of 5 and the content of 0.2 wt%, washing and drying the commercial melamine sponge to obtain the sponge with the micro-nano structure;
and then soaking the obtained sponge with the micro-nano structure into a prepared 0.05 wt% stearic acid solution with the volume of 100mL, and cleaning and drying to obtain the emulsion separation super-hydrophobic sponge with S-MH loaded on the surface.
The scanning electron micrograph of the emulsion-separated superhydrophobic sponge prepared in the example is shown in fig. 1, and the water contact angle is shown in fig. 2. And cutting the prepared emulsion separation super-hydrophobic sponge into proper size, putting the cut sponge into the middle of a column tube, and ensuring that no gap exists between the sponge and the column tube.
100mL of a toluene-in-water emulsion containing 0.01g/L cetyltrimethylammonium bromide (CTAB) prepared by a high shear emulsifying machine was poured over the column tube, and the volume ratio of water to oil in the emulsion was 1/50. After the emulsion is poured from the upper part of the column tube, the emulsion can flow through the emulsion separation super-hydrophobic sponge arranged in the middle part under the action of gravity, the separated toluene is absorbed in the sponge, and the separated water directly flows to the lower part through the sponge, as shown in figure 3, the oil-water separation efficiency is 99.5%.
The emulsion separation super-hydrophobic sponge is repeatedly used for more than 10 times after being fully washed and dried by ethanol, and the oil-water separation efficiency is not lower than 99%. Therefore, the emulsion separation super-hydrophobic sponge has good recycling performance.
Example 2
Preparing 100mL of 0.2M NaOH aqueous solution, adding Cetyl Trimethyl Ammonium Bromide (CTAB) with the mass of 3% of the theoretically prepared magnesium hydroxide, and stirring for 10 min; then, 25mL of a 0.4M magnesium chloride solution prepared was slowly added dropwise to the aqueous NaOH solution containing CTAB. After the reaction is finished, continuously aging the mother liquor for 3 hours under the stirring state; after aging, the product is washed by deionized water for many times, then dried in an oven at 120 ℃ for 3 hours, ground and sieved to obtain CTAB-containing nano-scale magnesium hydroxide particles (C-MH).
Firstly, soaking commercial polyurethane sponge into 100mL of polyacrylic acid aqueous solution with the pH value of 1 and the content of 0.1 wt%, wringing out the polyacrylic acid aqueous solution, then soaking the sponge into 100mL of chitosan dispersion with the pH value of 5 and the content of 0.5 wt%, wringing out the chitosan dispersion, soaking the sponge into ultrapure water, then soaking the sponge into 100mL of magnesium hydroxide suspension with the pH value of 5 and the content of 0.1 wt%, washing and drying the suspension to obtain the sponge with a micro-nano structure;
and then soaking the obtained sponge with the micro-nano structure into a prepared 0.01 wt% stearic acid solution with the volume of 100mL, and cleaning and drying to obtain the emulsion separation super-hydrophobic sponge with the surface loaded with C-MH.
And cutting the prepared emulsion separation super-hydrophobic sponge into proper size, putting the cut sponge into the middle of a column tube, and ensuring that no gap exists between the sponge and the column tube.
100mL of a toluene-in-water emulsion containing 0.02g/L Sodium Dodecylbenzenesulfonate (SDS) prepared by a high-speed shearing emulsifier was poured into the column tube at the upper portion thereof, and the volume ratio of water to oil in the emulsion was 1/100. After the emulsion is poured from the upper part of the column tube, the emulsion can flow through the emulsion separation super-hydrophobic sponge arranged in the middle part under the action of gravity, the separated toluene is absorbed in the sponge, and the separated water directly flows to the lower part through the sponge, as shown in figure 4, the oil-water separation efficiency is 99.2%.
The emulsion separation super-hydrophobic sponge is repeatedly used for more than 10 times after being fully washed and dried by ethanol, and the oil-water separation efficiency is not lower than 98.7 percent. Therefore, the emulsion separation super-hydrophobic sponge has good recycling performance.
Claims (6)
1. A preparation method of a super-hydrophobic sponge with an emulsion separation function is characterized by comprising the following steps:
(1) firstly, adding a certain amount of surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) or Sodium Dodecyl Benzene Sulfonate (SDBS) into a sodium hydroxide aqueous solution, wherein the addition amount of the surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) or the Sodium Dodecyl Benzene Sulfonate (SDBS) is 2-4% of the theoretical yield of magnesium hydroxide; then, slowly dripping a magnesium chloride solution into the sodium hydroxide aqueous solution containing the surfactant, wherein the molar ratio of sodium hydroxide to magnesium chloride is 1: 2; after the reaction is finished, continuously aging the mother liquor for 3 hours under the stirring state; after aging, washing the product for many times by deionized water, then drying for 3 hours at 120 ℃, grinding and sieving to obtain nano magnesium hydroxide particles;
(2) preparing a polyacrylic acid solution, a chitosan solution and a suspension containing nano magnesium hydroxide particles with certain concentration and pH value, stirring for 6-24 h, sequentially immersing commercial polymer sponge into the polyacrylic acid solution, the chitosan solution and the suspension containing the nano magnesium hydroxide particles, washing and drying to obtain sponge with a micro-nano layered structure;
(3) and soaking the dried sponge with the micro-nano layered structure by using a low surface energy surfactant stearic acid solution with the concentration of 0.005-0.1M, and drying to obtain the super-hydrophobic sponge for realizing emulsion separation.
2. The method for preparing the superhydrophobic sponge with the emulsion separation function according to claim 1, wherein the commercial polymer sponge in the step (2) is melamine sponge or polyurethane sponge with characteristics of low cost, light weight, small pore size, good elasticity and the like, and the porosity is 98.5-99.5%.
3. The method for preparing a superhydrophobic sponge having an emulsion separation function according to claim 1, wherein the pH of the aqueous solution of polyacrylic acid in the step (2) is 1 and the concentration is 0.1 wt%.
4. The method for preparing a superhydrophobic sponge having an emulsion separation function according to claim 1, wherein the solution of chitosan in the step (2) has a pH of 5 and a concentration of 0.5 wt%.
5. The method for preparing a superhydrophobic sponge with emulsion separation function according to claim 1, wherein the magnesium hydroxide suspension in the step (2) has a pH of 10 and a concentration of 0.05 to 0.5 wt%.
6. The method for preparing the superhydrophobic sponge with the emulsion separation function according to claim 1, wherein the step (3) of treating the sponge with the micro-nano layered structure with the surfactant with low surface energy comprises directly soaking the sponge in a stearic acid solution for 2-8 hours.
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| CN101376511A (en) * | 2007-11-23 | 2009-03-04 | 清华大学深圳研究生院 | Preparation of nano magnesium hydrate |
| CN105778149A (en) * | 2016-03-30 | 2016-07-20 | 天津大学 | Preparation method for super-hydrophobic polymeric sponge |
| US10131556B1 (en) * | 2018-04-20 | 2018-11-20 | King Saud University | Hydrophobic nanoparticle compositions for crude oil collection |
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|---|---|---|---|---|
| CN101376511A (en) * | 2007-11-23 | 2009-03-04 | 清华大学深圳研究生院 | Preparation of nano magnesium hydrate |
| CN105778149A (en) * | 2016-03-30 | 2016-07-20 | 天津大学 | Preparation method for super-hydrophobic polymeric sponge |
| US10131556B1 (en) * | 2018-04-20 | 2018-11-20 | King Saud University | Hydrophobic nanoparticle compositions for crude oil collection |
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| 王伟.阻燃性油水分离泡沫状材料的制备及其性能研究.《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑》.2018,(第1期),第B016-25页. * |
| 阻燃性油水分离泡沫状材料的制备及其性能研究;王伟;《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑》;20180115(第1期);第36页第3.2.3、3.2.4节，第37页第3.3.1节，第40页第3.3.4节 * |
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