CN115340151A - Membrane extraction method for separating ethanol from ethanol high-salt wastewater - Google Patents
Membrane extraction method for separating ethanol from ethanol high-salt wastewater Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 43
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- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
Abstract
The invention discloses a self-driven low-energy-consumption membrane extraction method for separating ethanol from ethanol high-salinity wastewater. In the membrane component, the hydrophobic and organophilic porous or thin-layer composite membrane material divides the component into two independent chambers, and simultaneously wastewater containing high-concentration ethanol and salt enters one of the chambers from a feeding tank in a cross flow manner and circulates under the driving of a circulating pump; in the other chamber, water is used as the receiving liquid, circulating. The ethanol gradually passes through the membrane and enters the receiving liquid under the drive of the pressure difference caused by the concentration difference and the flow difference on the two sides of the membrane, and the salt is completely intercepted by the hydrophobic membrane, so that the high-efficiency separation and recovery of the ethanol are realized. The method is simple to operate, only operates under low pressure/no pressure, and has lower energy consumption and higher separation purity compared with other separation modes. The ethanol solution separated by the method can be used for a denitrification carbon source supplement in sewage treatment and further purification and utilization, effectively improves the reuse rate of the wastewater, and is simple and easy to implement.
Description
Technical Field
The invention relates to the technical field of ethanol wastewater recycling, in particular to a self-driven low-energy-consumption membrane extraction method for separating ethanol from ethanol high-salt wastewater.
Background
The industrial production discharges a large amount of industrial wastewater containing high-concentration organic and inorganic pollutants, and the separation and extraction of valuable organic resources from the wastewater is an important way for the resource utilization of sewage, thereby not only being beneficial to realizing the high-value utilization of the wastewater, but also effectively reducing the difficulty and the cost of the subsequent wastewater treatment. Taking ethanol high-salt wastewater from food industry, medical and health industry and other industries as an example, the wastewater contains a large amount of ethanol and inorganic salt and has strong toxic action on microorganisms in biological treatment. In addition, ethanol is a valuable industrial feedstock, and has significant environmental and economic value for its separation and recovery from wastewater.
At present, the technologies for recovering ethanol from ethanol high-salt wastewater mainly comprise a distillation method, a pervaporation method and the like. The distillation method is an operation method for evaporating ethanol and condensing and recovering ethanol by precisely controlling the temperature by utilizing the difference of boiling points between ethanol and a solvent. Chinese patent (CN 202111074945) develops a device for recovering ethanol from ethanol waste liquid by using a distillation method, the heating speed and heat loss in the distillation process are effectively improved, but high temperature is continuously provided in the separation process of the ethanol waste liquid, the device is matched with condensation operation, the device also faces serious scaling problem when waste water with too high concentration of inorganic salt is treated, the process is complex, and the occupied area is large. The pervaporation method artificially creates vacuum or near vacuum conditions at the downstream of the membrane, so that the chemical potential of the feed liquid generates larger difference at the upstream and the downstream of the membrane, and further, the selective separation technology is realized by utilizing the difference of the affinity and the mass transfer resistance of the membrane to different components in the feed liquid. Chinese patent (CN 202110127875) developed a silica-coated graphene oxide nanocomposite-filled polydimethylsiloxane membrane material, which realizes high-flux pervaporation of ethanol solution, but in order to maintain the chemical potential gradient of ethanol at both sides of the membrane, a vacuum receiving environment is usually continuously created at the permeation side, and a higher temperature is maintained at the raw material side, which all require a large amount of extra energy to be consumed. Whether requiring large steady heat source inputs or consuming large amounts of energy, are obstacles to these techniques for separating ethanol from ethanol-rich wastewater.
Therefore, those skilled in the art are dedicated to search whether the pressure difference caused by the ethanol concentration difference and the flow difference on two sides of the membrane can be utilized to separate ethanol from ethanol high-salinity wastewater, and develop a self-driven membrane extraction ethanol separation method with low energy consumption. According to the invention, water is used as receiving liquid, pressure difference caused by concentration difference and flow difference of ethanol on two sides of the membrane is used as driving force, and the ethanol is separated from the ethanol high-salt wastewater by utilizing the difference of mass transfer performance of ethanol and salt in the hydrophobic and organophilic membrane. Compared with a distillation method which is driven by a heat source and a pervaporation method which is driven by a continuous vacuum environment, the membrane extraction method which takes the pressure difference caused by the concentration difference and the flow difference of ethanol at two sides of the membrane as the main driving force is a more green technology with lower energy consumption.
Disclosure of Invention
In order to solve the defects of the prior ethanol separation technology, the invention provides a membrane extraction method for separating ethanol from ethanol high-salt wastewater. The method is green and environment-friendly, and overcomes the defects that the prior separation method needs to consume a large amount of energy or extra chemical resources and the like. The regulation of the ethanol separation rate and the complete interception of salt can be realized by regulating and controlling the system operation parameters, the membrane thickness and the membrane material, the purity of the separated product is high, and the method can be used for various purposes such as wastewater pretreatment, carbon source supplement of sewage plants and the like.
The invention provides a membrane extraction method for separating ethanol from ethanol high-salt wastewater, which comprises the following steps:
fixing a hydrophobic and hydrophilic organic porous membrane or a thin-layer composite membrane in a membrane assembly, dividing the membrane assembly into two independent chambers, connecting the membrane assembly with a feed tank by using a pipeline, and respectively adding a circulating pump, a valve and a pressure gauge in the pipeline;
step 4, adjusting the circulating pump, setting the flow, flow speed and transmembrane pressure of the receiving liquid and the feeding liquid, and starting the circulating pump;
and 6, optionally, determining whether the membrane material is replaced, and replacing the receiving liquid to start the next operation.
Furthermore, the salt concentration range of the ethanol high-salt wastewater in the step is 0-50 g/L, the ethanol concentration range is 1-10 g/L, and the surface tension of the wastewater after insoluble substances are removed is more than 60mN/m (20 ℃).
Further, the pH range of the wastewater is 5-8, the temperature is 25 +/-5 ℃, and the stirring speed is 100-500 r/min.
Further, in the step 2, the water contact angle of the hydrophobic and organophilic porous or thin-layer composite membrane is larger than 110 degrees, and the ethanol contact angle is smaller than 40 degrees.
Furthermore, the aperture of the hydrophobic and organophilic porous membrane is 0.1-1 μm, and the aperture of the thin-layer composite membrane is 0-0.1 μm.
Further, the hydrophobic and organophilic porous membrane or thin-layer composite membrane material is one or more of polyvinylidene fluoride, polypropylene, polyacrylonitrile, polytetrafluoroethylene, polymethyl methacrylate, polydimethylsiloxane and cyclodextrin.
Further, the hydrophobic and organophilic porous membrane is prepared by a phase inversion method or an electrostatic spinning method, and the hydrophobic and organophilic thin-layer composite membrane is a composite of a nanofiber membrane and a thin-layer membrane prepared by the electrostatic spinning method.
Furthermore, the water flow mode in the membrane module is cross flow, and the effective membrane area is 20-100 cm 2 The component is made of stainless steel or polytetrafluoroethylene.
Further, the pH value of the receiving liquid is 2-12, and the temperature is 15-35 ℃.
Further, the operating parameters are: the flow rate of the feeding liquid and the receiving liquid is 0.1-10 cm/s, the flow is 0.1-50L/h, and the transmembrane hydraulic pressure is 0-20 kPa.
The membrane extraction method for separating ethanol from ethanol high-salt wastewater is applied to the fields of wastewater treatment, wastewater recycling and the like.
The principle of the technical scheme of the invention is as follows:
the species spontaneously diffuse from the high concentration region to the low concentration region until uniformly distributed, and there is a significant difference in the diffusion rates of different species in the same medium. The hydrophobic and organophilic selective permeation extraction membrane is used for separating the ethanol high-salt wastewater from the receiving liquid, because the concentration of ethanol and salt in the wastewater side is far higher than that of the receiving liquid side, and simultaneously, under the action of hydraulic pressure difference caused by flow difference, ethanol molecules and salt can diffuse to the receiving liquid side, but the hydrophobic and organophilic membrane can block the passage of water and further block the transmembrane of the salt, and the ethanol can gradually enter the receiving liquid through the transmembrane in a dissolving-diffusing process, so that the separation of the ethanol and the salt is realized. Therefore, the method does not need to consume additional energy and chemical resources, and can realize the regulation and control of the ethanol separation efficiency.
The invention has the beneficial technical effects that:
(1) The method is simple, does not need complex equipment, has stronger adaptive range to temperature and pressure, occupies small area and is easy to realize automatic control; better ethanol separation effect can be obtained; by regulating and controlling the selective permeation extraction membrane and the operation parameters, continuous and stable transmembrane of the ethanol and complete interception of salt can be realized.
(2) The invention is green and energy-saving; extra energy and chemical resources are not required to be consumed; water is used as receiving liquid, only pressure difference caused by concentration difference and flow difference of ethanol on two sides of the membrane is used as mass transfer driving force, mass transfer efficiency of the ethanol is controllable, the problem of high cost in the previous ethanol separation process is solved, and the green development concept is met.
(3) The method has wide applicability; the ethanol can be extracted from ethanol high-salt wastewater with different concentrations, and various water bodies such as surface water, tap water, secondary effluent of a sewage plant and the like can be used as receiving liquid.
Drawings
FIG. 1 is a schematic diagram of an apparatus used in a preferred embodiment of the present invention; wherein 1 is a wastewater storage tank, 2 is a circulating pump, 3 is a pressure gauge, 4 is a membrane material, 5 is a membrane component, 6 is a pipeline valve, and 7 is a receiving liquid storage tank.
FIG. 2 is a surface topography (SEM) and Atomic Force Microscopy (AFM) of a porous polyvinylidene fluoride nanofiber membrane used in a preferred embodiment of the present invention;
FIG. 3 is a top and bottom surface topography (SEM) and surface Atomic Force Microscopy (AFM) of a thin film composite membrane used in a preferred embodiment of the invention;
FIG. 4 shows the ethanol separation (ethanol transmembrane flux and salt rejection) achieved by a preferred embodiment of the present invention;
FIG. 5 shows the ethanol separation (ethanol transmembrane flux and salt rejection) achieved by a preferred embodiment of the invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
In the drawings, the size and thickness of each component shown are arbitrarily illustrated, and the present invention is not limited to the size and thickness of each component. The thickness of the components may be exaggerated where appropriate in the figures to improve clarity.
FIG. 1 is a schematic diagram of an apparatus used in a preferred embodiment of the present invention; fig. 2 is a surface topography (SEM) and a surface Atomic Force Microscope (AFM) of a porous polyvinylidene fluoride nanofiber membrane used in the method of the present invention, and fig. 3 is a top and bottom surface topography (SEM) and a surface Atomic Force Microscope (AFM) of a thin-layer composite membrane used in the method of the present invention.
Example 1:
a membrane extraction method for separating ethanol from ethanol high-salt wastewater comprises the following steps:
step 4, regulating the flow and flow rate of the receiving liquid and the feeding liquid in the membrane module, and measuring the hydraulic transmembrane pressure at two sides of the membrane, wherein specific parameters are listed in table 1;
and 6, replacing the wastewater and the receiving liquid, and starting the next separation operation.
FIG. 1 is a schematic view of the apparatus used in the present embodiment, and it can be seen that the method has a simple structure, a small floor space and is easy to operate; fig. 2 is a surface topography (SEM) and Atomic Force Microscopy (AFM) of the hydrophobic and organophilic nanofiber polyvinylidene fluoride membrane used in this example, with micron-sized pore sizes providing large free volume for ethanol molecules to pass through the membrane and roughness large enough to render the membrane excellent in hydrophobicity for complete salt entrapment. In addition, the strong affinity between ethanol and polyvinylidene fluoride allows ethanol to rapidly cross membranes through a dissolution-diffusion process.
Sampling and detecting the conductivity change and the ethanol concentration of the receiving solution at 1h, 3h, 6h, 12h and 24h respectively; FIG. 4 is a calculated Ethanol flux (Ethanol flux, g m) 2 h -1 ) And Salt rejection (Salt rejection,%), calculated as follows:
wherein V r (L) is the volume of the receiving liquid, C r t (mg L -1 ) Is the concentration of ethanol in the receiving solution at time t (h), A (m) 2 ) Is the effective area of the membrane material, C f，NaCI (mg L -1 ) And C r，NaCI (mg L -1 ) The concentrations of sodium chloride in the wastewater and the receiving solution are respectively. Under different pressure conditions, the left-side bar graph represents the ethanol flux, the right-side bar graph represents the salt rejection rate, and as can be seen from the graph, the system can achieve 100% of the salt rejection rate under the hydraulic transmembrane pressure of 0-9kPa, and meanwhile, the ethanol flux is increased along with the increase of the hydraulic pressure; the ethanol transmembrane flux is 34.7g m at 9kPa 2 h -1 (ii) a After 24h, the conductivity of the receiving liquid still maintains the initial level, the concentration of the ethanol is higher, and the receiving liquid can be used for supplementing a carbon source in a sewage plant and the like.
TABLE 1 transmembrane pressure, flow rate and flow rate of feed and receiving fluids during operation
Example 2:
a membrane extraction method for separating ethanol from ethanol high-salt wastewater comprises the following steps:
step 4, regulating the flow and flow rate of the receiving liquid and the feeding liquid in the membrane module, and measuring the hydraulic transmembrane pressure at two sides of the membrane, wherein specific parameters are listed in table 1;
and 6, replacing the wastewater and the receiving liquid, and starting the next separation operation.
FIG. 3 is a top and bottom surface topography (SEM) and surface Atomic Force Microscopy (AFM) of the thin composite film used in this example, with polyvinylidene fluoride providing sufficiently large pore size and hydrophobicity at the top surface; on the bottom side, a thin layer of relatively dense polydimethylsiloxane ensures excellent salt rejection properties of the membrane.
Sampling and detecting the conductivity change and the ethanol concentration of the receiving solution at 1h, 3h, 6h, 12h and 24h respectively; FIG. 5 is a graph of calculated ethanol flux and salt rejection; the left bar graph shows the ethanol flux and the right bar graph shows the salt rejection under different pressure conditions, and it can be seen from the graph that the ethanol transmembrane flux is 6.12g m at 9kPa 2 h -1 After 24h, the receiver conductivity remained at the initial level with a salt rejection of 100%.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (9)
1. A membrane extraction method for separating ethanol from ethanol high-salt wastewater is characterized by comprising the following steps:
step 1, removing insoluble suspended matters from ethanol high-salt wastewater to be separated, introducing the ethanol high-salt wastewater into a feeding tank, adjusting the pH of the wastewater to a proper range by using acid and alkali, adjusting the temperature of the wastewater, and covering and stirring the wastewater to uniformly mix the wastewater;
fixing a hydrophobic and hydrophilic organic porous membrane or a thin-layer composite membrane in a membrane assembly, dividing the membrane assembly into two independent chambers, connecting the membrane assembly with a feed tank by using a pipeline, and respectively adding a circulating pump, a valve and a pressure gauge in the pipeline;
step 3, introducing the receiving liquid into a receiving liquid tank, adjusting the pH value of the receiving liquid, and connecting the receiving liquid with the membrane module in the same way;
step 4, adjusting the circulating pump, setting the flow, flow speed and transmembrane pressure of the receiving liquid and the feeding liquid, and starting the circulating pump;
step 5, monitoring the conductivity of the receiving liquid in real time by using a conductivity meter, sampling and detecting the concentration of ethanol in the receiving liquid at regular time, and determining the operation ending time according to the use requirement;
and 6, optionally, determining whether the membrane material is replaced, and replacing the receiving liquid to start the next operation.
2. The membrane extraction method for separating ethanol from ethanol high-salt wastewater as claimed in claim 1, wherein in the step 1, the salt concentration of the ethanol high-salt wastewater is in the range of 0 to 50g/L, the ethanol concentration is in the range of 1 to 10g/L, and the surface tension of the wastewater after removing insoluble substances is more than 60mN/m (20 ℃).
3. The membrane extraction method for separating ethanol from ethanol high-salt wastewater as claimed in claim 1, wherein in the step 1, the pH of the wastewater ranges from 5 to 8, the temperature is 25 +/-5 ℃, and the stirring speed is 100 to 500r/min.
4. The membrane extraction method for separating ethanol from ethanol high-salt wastewater as claimed in claim 1, wherein in the step 2, the hydrophobic and organophilic porous or thin layer composite membrane has a water contact angle of more than 110 ° and an ethanol contact angle of less than 40 °.
5. The membrane extraction method for separating ethanol from ethanol high-salt wastewater as claimed in claim 1, wherein in the step 2, the pore diameter of the hydrophobic and organophilic porous membrane is 0.1-1 μm, and the pore diameter of the thin-layer composite membrane is 0-0.1 μm.
6. The membrane extraction method for separating ethanol from ethanol high-salt wastewater according to claim 1, wherein in the step 2, the water flow mode in the membrane modules is cross flow, and the effective membrane area of a single membrane module is 20-100 cm 2 The component is made of stainless steel or polytetrafluoroethylene.
7. The membrane extraction method for separating ethanol from ethanol high-salt wastewater as claimed in claim 1, wherein in the step 3, the pH of the receiving solution is 2-12, and the temperature is 15-35 ℃.
8. The membrane extraction process for separating ethanol from ethanol high-salt wastewater according to claim 1, wherein in the step 4, the operation parameters are as follows: the flow velocity of the feeding liquid and the receiving liquid is 0.1-10 cm/s, the flow is 0.1-50L/h, and the transmembrane hydraulic pressure is 0-20 kPa.
9. The use of a membrane extraction method for separating ethanol from ethanol-rich wastewater as claimed in any one of claims 1 to 8 in wastewater treatment and wastewater reclamation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58180442A (en) * | 1982-04-19 | 1983-10-21 | Asahi Chem Ind Co Ltd | Separation and concentration method of ethanol from aqueous solution thereof |
| CN101559993A (en) * | 2009-05-19 | 2009-10-21 | 新奥科技发展有限公司 | Method for removing trace alcohol in organic wastewater |
| CN102228801A (en) * | 2011-05-16 | 2011-11-02 | 何涛 | Hydrophobically modified distillation membrane material of high throughout and high salt rejection rate and application thereof |
| CN104609621A (en) * | 2013-11-01 | 2015-05-13 | 中国石油化工股份有限公司 | High-salt waste water treatment method |
-
2022
- 2022-08-31 CN CN202211052854.5A patent/CN115340151B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58180442A (en) * | 1982-04-19 | 1983-10-21 | Asahi Chem Ind Co Ltd | Separation and concentration method of ethanol from aqueous solution thereof |
| CN101559993A (en) * | 2009-05-19 | 2009-10-21 | 新奥科技发展有限公司 | Method for removing trace alcohol in organic wastewater |
| CN102228801A (en) * | 2011-05-16 | 2011-11-02 | 何涛 | Hydrophobically modified distillation membrane material of high throughout and high salt rejection rate and application thereof |
| CN104609621A (en) * | 2013-11-01 | 2015-05-13 | 中国石油化工股份有限公司 | High-salt waste water treatment method |
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