Simple oil-water separation device based on novel separation membrane technology
Patent Information
- Application Number
- CN202611326846.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-30
- Publication Date
- 2026-10-20
AI Technical Summary
然而，该技术仍存在不足：膜材料易受油污粘附和其他颗粒状杂质黏附导致通量衰减或直接堵塞，即膜污染问题突出；部分亲油或亲水膜在复杂水质下稳定性不足；此外，高性能膜材料制备成本偏高、废弃膜的销毁容易造成二次污染和膜清洗困难等问题也日益突出
其一，采用工业级醋酸纤维素为原料，通过静电纺丝工艺制备纳米纤维膜，原料易得、成本低廉且膜本身可自然降解，符合绿色发展理念；纺丝工艺简单可控，便于规模化生产，可进一步压缩成本，使得产品更容易普及；其二，经KOH/水/甲醇体系脱乙酰化改性后，膜片亲水性显著提升，可在重力驱动下实现矿物油与乳化油的高效截留，无需外加压力与化学药剂，能耗低且无二次污染；其三，装置采用滤袋层、亲水分离膜与单孔布水层的模块化组合结构，组装简便、运行稳定，三层膜交错叠放进一步增强了分离精度与抗污染能力；其四，膜片可通过碱液浸泡再生，经水洗、干燥后重复使用，有效降低运行维护成本；其五，整体装置结构简易、占地小，适用于含油废水的现场快速处理与小规模净化，具有良好的实用价值与推广前景。
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of industrial wastewater treatment technology, and in particular relates to the preparation and application of a simple oil-water separation device based on a novel separation membrane technology. Background Technology
[0002] With the increasing frequency of industrial production, transportation, and marine development activities, oil pollution has become a global environmental problem. During the extraction, transportation, storage, and use of petroleum and its products, leaks, discharges, or accidents can enter water bodies and soil, posing a serious threat to ecosystems. Oil spills form films on the water surface, hindering oxygen exchange and sunlight penetration, leading to the suffocation and death of aquatic organisms. Simultaneously, toxic substances such as polycyclic aromatic hydrocarbons can accumulate through the food chain, harming human health. In recent years, although countries have strengthened their regulatory and emergency response capabilities, oil pollution still occurs frequently, and its remediation is difficult and time-consuming, urgently requiring high attention from the entire society. Furthermore, my country is an oil-poor country, heavily reliant on imported mineral oil resources. Therefore, the market urgently needs an efficient, green, convenient, and low-cost oil-water separation technology for oil pollution treatment and the recovery of high-value mineral oils.
[0003] While there are many existing oil spill remediation technologies, significant shortcomings remain: physical adsorption methods suffer from high material costs, easy saturation, and limited effectiveness in removing dissolved oil; chemical dispersion methods may introduce secondary pollution and damage aquatic ecosystems; and biodegradation methods are time-consuming, highly dependent on environmental conditions, and ill-suited for handling sudden large-scale oil spills. Furthermore, most technologies generally experience reduced efficiency in complex water conditions and high-concentration oil spills, resulting in low resource recovery rates.
[0004] Membrane separation technology has demonstrated significant advantages in oil pollution control: it achieves efficient oil-water separation through pore size sieving or interfacial selectivity, with low energy consumption, simple operation, no need for chemical reagents, avoidance of secondary pollution, and continuous operation at room temperature, making it suitable for large-scale treatment of oily wastewater. However, this technology still has shortcomings: membrane materials are susceptible to oil adhesion and the adhesion of other particulate impurities, leading to flux attenuation or direct clogging, i.e., membrane fouling is a prominent problem; some oleophilic or hydrophilic membranes lack stability under complex water conditions; in addition, the high cost of manufacturing high-performance membrane materials, the potential for secondary pollution from the disposal of waste membranes, and the difficulty of membrane cleaning are also increasingly prominent issues. In summary, these shortcomings greatly limit its widespread application in the industrial field. Summary of the Invention
[0005] To address the aforementioned problems, this invention proposes a simple oil-water separation device based on novel separation membrane technology. A technological breakthrough is achieved through the combination of high-performance materials and a simple device. The specific solution is as follows: A simple oil-water separation device based on a novel separation membrane technology, characterized in that the assembly of the device includes the following steps: S1. A certain amount of industrial grade cellulose acetate is mixed and dissolved in acetic acid / dichloromethane solvent to obtain a spinning solution; a certain amount of spinning solution is taken with a syringe, and the syringe is pushed slowly and evenly under the stable voltage of the electrospinning machine to spin single needles on aluminum foil. S2. Take three standard-sized membranes and place them in plastic petri dishes. Slowly pour in an appropriate amount of deacetylation solution and deacetylate them in a ventilated place for a certain period of time. After rinsing with water, dry them in a fume hood to obtain the hydrophilic membrane. S3. The three prepared hydrophilic membranes are stacked together in an alternating manner, soaked in water, clamped with hollow rubber sheets, and pressed to obtain the required cellulose acetate-based hydrophilic membrane sheet. Then, the cellulose acetate-based hydrophilic membrane sheet and the filter screen are fixed in the hollow membrane column in sequence to complete the middle section of the device, namely the filter bag layer and oil-water separation membrane of the core functional block. S4, the upper section of the device with an inlet and a water collection layer and the lower section of the device with a single-hole water distribution layer, a base and an outlet are riveted together with screws, and connected to an external water pump and a storage tank through a conduit, which is a simple oil-water separation device based on a new separation membrane technology.
[0006] Furthermore, the aforementioned simple oil-water separation device based on novel separation membrane technology is characterized in that the cellulose acetate substrate is specifically prepared as follows: 10wt% of industrial-grade cellulose acetate was mixed and dissolved in a solution of acetic acid / dichloromethane with a volume ratio of 2:1 to prepare a spinning solution. Using a 20mL syringe, 15mL of the spinning solution was taken and spun on aluminum foil using an electrospinning machine at a voltage of 22kV and -1.5kV and a feed speed of 0.5mm / min. Furthermore, the aforementioned simple oil-water separation device based on novel separation membrane technology is characterized in that the specific modification process of the cellulose acetate-based hydrophilic membrane and the oil-water separation membrane is as follows: A 15x15cm cellulose acetate membrane is laid flat in a plastic petri dish. An appropriate amount of deacetylation solution is slowly poured into the membrane until it is completely submerged. The deacetylation reaction is carried out in a ventilated place for 12 hours. Afterward, the residual deacetylation reagent is washed away with water, and then the membrane is dried in a fume hood for 24 hours to obtain the desired hydrophilic cellulose acetate membrane. Furthermore, the aforementioned simple oil-water separation device based on novel separation membrane technology is characterized in that the deacetylation reagent is: A mixed solution of 0.1-0.5 mol / L KOH, with a water / methanol solution in a volume ratio of 1:1; Furthermore, the aforementioned simple oil-water separation device based on novel separation membrane technology is characterized in that the rubber sheet used is a hollow circular sheet with a diameter of 20cm, with a central contact area of 1.5-2.5dm² for contact with wastewater. 2 Hollow holes; Furthermore, the simple oil-water separation device based on the novel separation membrane technology is characterized in that the filter screen used in the filter bag layer is a micron-sized nylon filter cloth; Furthermore, the simple oil-water separation device based on the novel separation membrane technology is characterized in that the single-hole filter hole of the water distribution layer is a circular hole with a diameter of 5cm. Furthermore, the simple oil-water separation device based on the novel separation membrane technology is characterized in that the spacing ratio of the top end of the water collection cavity layer, the filter bag layer, the oil-water separation membrane, the water distribution layer and the bottom end is 1-3:5:5:1-3. This invention also discloses a processing flow and subsequent membrane cleaning flow for the oil-water separation column, including the following steps: Preferably, the wastewater sample is pumped into the oil-water separation column by an external water pump at a rate of 0.5%-2% of the total cavity volume of the device. After the wastewater is naturally filtered through the membrane by gravity, the mineral oil and emulsified oil in the water can be quickly separated from the water. Moreover, thanks to the hydrophilicity of the membrane, the mineral oil and emulsion cannot be filtered through the membrane and are well retained, thus achieving the initial purification of the wastewater.
[0007] Preferably, the membrane is removed from the device, and the rubber sheets at both ends are removed. The membrane is first washed with hydrophilic and methanol 2-3 times. Then, without drying, it is soaked again in the deacetylation reagent for 0.5-2 hours, washed again with hydrophilic and methanol 2-3 times, and then dried in a ventilated place for 24 hours.
[0008] The present invention has the following beneficial effects: Firstly, the nanofiber membrane is prepared using industrial-grade cellulose acetate as raw material through electrospinning. The raw material is readily available and inexpensive, and the membrane itself is biodegradable, aligning with the concept of green development. The spinning process is simple and controllable, facilitating large-scale production and further reducing costs, making the product more widely available. Secondly, after deacetylation modification using a KOH / water / methanol system, the membrane's hydrophilicity is significantly enhanced, enabling efficient retention of mineral oil and emulsified oil under gravity, without the need for external pressure or chemical reagents, resulting in low energy consumption and no secondary pollution. Thirdly, the device employs a modular combination structure of filter bag layer, hydrophilic separation membrane, and single-pore water distribution layer, which is easy to assemble and operates stably. The staggered stacking of the three membrane layers further enhances separation accuracy and anti-fouling capabilities. Fourthly, the membrane can be regenerated by alkali immersion and reused after washing and drying, effectively reducing operating and maintenance costs. Fifthly, the overall device has a simple structure and small footprint, making it suitable for rapid on-site treatment and small-scale purification of oily wastewater, demonstrating good practical value and promising prospects for widespread application. Attached Figure Description
[0009] Figure 1 This is a physical drawing of the present invention; Figure 2 This is a diagram illustrating a practical application scenario of the present invention; Figure 3 The figures show the actual effects of this invention on mineral oil, emulsified oil, and mixed oil. Figure 4 The images show actual pictures of the membrane used in this invention, as well as comparison pictures of the old membrane before and after cleaning. Figure 5 This is a data table showing the data before and after processing according to the present invention. Detailed Implementation
[0010] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to embodiments and accompanying drawings: Example 1 First, mix 500mL of emulsified oil with 100mL of water to create a suspended wastewater environment with high oil content; 2.38 g of industrial-grade cellulose acetate was added to a homogeneous solution consisting of 10 mL of dichloromethane and 10 mL of acetic acid. After stirring at 300 rpm for 1 hour, the mixture was sonicated for 15 minutes to remove internal air bubbles, resulting in a homogeneous polymer spinning solution without obvious precipitates. Then, 15 mL of the spinning solution was drawn using a 20 mL syringe, fitted with a 21G needle, and aluminum foil was attached to the receiver. The distance between the spinneret and the rotating drum collecting device was adjusted to 15 cm. Subsequently, the spinning temperature and humidity were set to 25℃ and 50%, respectively, and the positive and negative voltages were adjusted to 18 kV and -2.5 kV, respectively. The syringe push rate was 0.5 mm / min. After spinning was complete, the spun cellulose acetate fiber membrane was removed. Add 2 mL of methanol to 8 mL of water and stir at 200 rpm for 10 min. Then add 0.251 g of sodium hydroxide and stir at 200 rpm for 10 min to successfully obtain the deacetylation reagent. Take a standard 15 x 15 cm membrane from the freshly spun material and place it in a volumetric plastic petri dish. Pour in the deacetylation reagent, ensuring the membrane is completely immersed. Cover the dish and react in a fume hood for 12 h. Wash 2-3 times with water and methanol respectively, and then react and dry in a fume hood for 24 h to obtain the desired hydrophilic membrane.
[0011] Next, a hollow rubber disc with a diameter of 20cm is used to clamp a standard hydrophilic membrane and fix it to the middle section of the membrane column. Then, a 20x20cm three-layer micron nylon mesh is fixed 15cm above the oil-water separation membrane. The upper and lower sections of the membrane column are then assembled and secured with four screws at the joint. After tightening, oily wastewater is continuously pumped in from the top at a rate of 15mL / min and continuously extracted from the bottom. The actual product and results are shown in the attached figure. Figure 2 As shown, the specific removal rate is as follows: Figure 5 As shown.
[0012] Example 2 For Example 1, 500 mL of mineral oil and 500 mL of water were mixed, and then methylene blue was added to stain the water. Other conditions remained unchanged. The resulting image is shown in the left figure of Figure 3. The specific removal rate is as follows: Figure 5 As shown; Example 3 For Example 1, 500 mL of mineral oil and 500 mL of water were mixed, then methylene blue was added to stain the water, and 10 g of granular calcium carbonate was added in addition. Other conditions remained unchanged, and the effect is shown in the middle figure of 3. Example 4 For Examples 1 and 2, 250 mL of mineral oil, 250 mL of emulsified oil, and 500 mL of water were mixed, and then methylene blue was added to stain the water. Other conditions remained unchanged, and the results were as follows: Figure 3 As shown in the right-hand figure, the specific removal rate is as follows: Figure 5 As shown.
[0013] Example 5: For Example 2, after the reaction was complete, the membrane was removed, and the rubber sheets at both ends were taken off. The membrane was first washed three times with hydrophilic and methanol solutions. Then, it was immersed again in the deacetylation reagent for 1 hour, followed by three more washes with hydrophilic and methanol solutions. Finally, it was placed in a ventilated area to dry for 24 hours. The resulting image is shown below. Figure 4 As shown.
[0014] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A simple oil-water separation device based on a novel separation membrane technology, characterized in that, The assembly of this device includes the following steps: S1. A certain amount of industrial grade cellulose acetate is mixed and dissolved in acetic acid / dichloromethane solvent to obtain a spinning solution; a certain amount of spinning solution is taken with a syringe, and the syringe is pushed slowly and evenly under the stable voltage of the electrospinning machine to spin single needles on aluminum foil. S2. Take three standard-sized membranes and place them in plastic petri dishes. Slowly pour in an appropriate amount of deacetylation solution and deacetylate them in a ventilated place for a certain period of time. After rinsing with water, dry them in a fume hood to obtain the hydrophilic membrane. S3, the three hydrophilic membranes are stacked together in an alternating manner, soaked in water, clamped with hollow rubber sheets and pressed to obtain the required cellulose acetate-based hydrophilic membrane sheet; then, the cellulose acetate-based hydrophilic membrane sheet and the filter screen are fixed in the hollow membrane column in sequence to complete the middle section of the device, namely the filter bag layer (2) and the oil-water separation membrane (3) of the core functional block. S4, the upper section of the device with inlet and water collection layer (1) and the lower section of the device with single-hole water distribution layer (4) and base and outlet are riveted together with screws and connected to an external water pump and storage tank through a conduit, which is a simple oil-water separation device based on a new separation membrane technology.
2. The simple oil-water separation device based on novel separation membrane technology according to claim 1, characterized in that, The cellulose acetate substrate is prepared as follows: 10 wt% of industrial-grade cellulose acetate was mixed and dissolved in a 1:1 volume ratio of acetic acid / dichloromethane solution to prepare a spinning solution. Using a 20 mL syringe, 15 mL of the spinning solution was taken and spun on aluminum foil using an electrospinning machine at a voltage of 22 kV and -1.5 kV and a feed speed of 0.5 mm / min.
3. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that, The specific modification process of the cellulose acetate-based hydrophilic membrane and the oil-water separation membrane (2) is as follows: A 15x15cm cellulose acetate membrane is laid flat in a plastic petri dish. An appropriate amount of deacetylation solution is slowly poured into the membrane until it is completely submerged. The deacetylation reaction is carried out in a ventilated place for 12 hours. Afterward, the residual deacetylation reagent is washed away with water, and then the membrane is dried in a fume hood for 24 hours to obtain the desired hydrophilic cellulose acetate membrane.
4. A simple oil-water separation device based on a novel separation membrane technology according to claim 3, characterized in that, The deacetylation reagent is: A mixed solution of 0.1-0.5 mol / L KOH, with a water / methanol solution in a volume ratio of 1:
1.
5. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that, The rubber sheet used is a hollow circle with a diameter of 20cm, with a center area of 1.5-2.5dm² for contact with sewage. 2 Hollow holes.
6. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that, The filter screen used in the filter bag layer is a micron-sized nylon filter cloth.
7. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that, The single-hole filter hole of the water distribution layer (4) is a circular hole with a diameter of 5cm.
8. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that, The spacing ratio of the top of the water collection cavity layer (1), the filter bag layer (2), the oil-water separation membrane (3), the water distribution layer (4), and the bottom is 1-3:5:5:1-3.
9. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that: The processing flow of the oil-water separation column includes the following steps: Wastewater samples are pumped into the oil-water separation column via an external water pump at a rate of 0.5%-2% of the total cavity volume of the device. After the wastewater passes through the membrane by gravity, mineral oil and emulsified oil in the water can be quickly separated from the water. Thanks to the hydrophilicity of the membrane, mineral oil and emulsion cannot pass through the membrane and are well retained, achieving preliminary purification of the wastewater.
10. A simple oil-water separation device based on a novel separation membrane technology according to claim 1, characterized in that, The cleaning of the cellulose acetate-based hydrophilic membrane after recycling includes the following steps: Remove the membrane from the device, remove the rubber sheets at both ends, and wash it 2-3 times with hydrophilic and methanol. Then, without drying, soak it again in the deacetylation reagent described in claim 3 for 0.5-2 hours, wash it 2-3 times with hydrophilic and methanol again, and then place it in a ventilated place to dry for 24 hours.