CN112442756B - Preparation method and application of porous fiber for oil-water separation - Google Patents
Preparation method and application of porous fiber for oil-water separation Download PDFInfo
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- CN112442756B CN112442756B CN201910799908.6A CN201910799908A CN112442756B CN 112442756 B CN112442756 B CN 112442756B CN 201910799908 A CN201910799908 A CN 201910799908A CN 112442756 B CN112442756 B CN 112442756B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- 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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
Abstract
The invention discloses a preparation method of porous fiber for oil-water separation and porous fiber prepared by the method, which comprises the following steps: s1, spinning a mixture containing polypropylene, polyethylene, a diluent and a nucleating agent to obtain nascent fiber; s2, cooling the nascent fiber to obtain a fiber filament; and S3, extracting the fiber filaments to obtain the porous fiber. The method has simple process and short production path, and the porous fiber prepared by the method has moderate aperture, high mechanical strength and excellent separation performance, is applied to oil-water separation, and has high separation efficiency. The invention also provides a device for oil-water separation, which has the advantages of simple structure, less power consumption, better removal effect on oil stains in sewage without adding any medicament, lower pollution and good application prospect in the field of oily sewage treatment.
Description
Technical Field
The invention relates to a preparation method of porous fiber for oil-water separation, a porous fiber material prepared by the method, application of the porous fiber material in oil-water separation, and a device for oil-water separation, belonging to the technical field of water treatment.
Background
Oil pollution, a common pollution, is extremely harmful to environmental protection and ecological balance. The range of producing the oily sewage is wide, and the oily sewage is produced in the processes of petroleum exploitation, petroleum refining, petrochemical industry, oil storage and transportation and the like. The oil-containing sewage in China has extremely high yield, more than 30 hundred million tons of oil-containing sewage are generated in oil fields and oil refining industries every year, the oil-containing sewage is one of the current industrial waste water which is difficult to treat, and along with the environmental protection requirement and the gradual strictness of energy conservation and consumption reduction, the oil-containing concentration of the discharged sewage specified in the comprehensive sewage discharge standard (GB 8978-1996) and the discharge standard of pollutants in the petroleum refining industry is less than 10ppm, which puts higher requirements on the sewage treatment capacity and the separation efficiency.
The coalescence-separation method is a physical oil-removing method, integrates gravity separation and coalescence technologies, and utilizes the characteristic of oil-water density difference to realize the separation process. The coalescence-separation device has the advantages of low power consumption, high separation efficiency, large operation elasticity and the like, when oily sewage passes through the coalescence-separation device, oil drops interact with the coalescence material, due to lipophilicity of the surface of the material, the oil drops and the surface of the material form a continuous oil film with a certain thickness, when subsequent oil drops pass through the surface, a liquid-sandwiched layer is formed between the oil drops and the layer film, the liquid drops deform and thin gradually in the liquid discharge process, the liquid film breaks when reaching a critical value, the two liquid drops are fused and grow up, the small oil drops are gradually fused and become large oil drops, and along with traction force of water flow, the large oil drops break away from the adsorption of the coalescence material to realize falling off and enter an oil layer under the action of buoyancy to be separated. The technical key point of the aggregation method for removing oil is the aggregation material which can be divided into porous materials, fiber materials, granular materials and the like, wherein the fiber materials can be made into materials with smaller diameter and larger surface area, and the aggregation method can have obvious oil removing efficiency.
The coalescence process mainly depends on the blocking and diffusion effects, and oil drops can be captured by the material under the action of Van der Waals attractive force only when moving to the surface close to the material, so that the action is only tied to the outer surface, the larger the outer surface, the higher the probability that the oil drops are close to the material and attached to the material, the more remarkable influence of the surface area of the material on the coalescence effect of the oil drops is, the surface area of the fiber material on the smooth surface can be improved by adopting a method of reducing the diameter, but the actual operation is greatly difficult due to the excessively small diameter of the coalescence material, and therefore, the more ideal method is to increase the roughness of the surface of the material so as to achieve the purpose of improving the surface area.
Disclosure of Invention
The invention aims to provide a preparation method of porous fiber for oil-water separation according to the defects in the prior art, oleophylic resin is made into a fiber material with porous surface through a thermal induced phase separation method (TIPS), and the roughness and the surface area of the surface are increased.
According to an aspect of the present invention, there is provided a method for preparing porous fiber for oil-water separation, comprising the steps of:
s1, spinning a mixture containing polypropylene, polyethylene, a diluent and a nucleating agent to obtain nascent fibers;
s2, cooling the nascent fiber to obtain a fiber filament;
and S3, extracting the fiber filaments to obtain the porous fiber for oil-water separation.
According to some embodiments of the invention, said step S1 comprises:
1A, melting and defoaming a mixture containing polypropylene, polyethylene, a diluent and a nucleating agent to obtain a spinning solution;
and 1B, conveying the spinning solution to a spinning nozzle, and extruding through the spinning nozzle to obtain nascent fibers.
According to the preferred embodiment of the invention, in the mixture, the polypropylene accounts for 17-85.5% by mass, the polyethylene accounts for 1-13.5% by mass, the nucleating agent accounts for 0.1-5% by mass, and the balance is the diluent. The fiber prepared in the mass ratio range has good mechanical property and uniform surface pore distribution.
According to the preferred embodiment of the present invention, the polypropylene resin has a melt index of 0.1-100g/10min, and the polypropylene resin with this melt index range has good flowability, processability and mechanical properties, and the melt index test condition is that the temperature is 230 ℃ and the load weight is 2.16 kg.
According to a preferred embodiment of the invention, the polyethylene is a high density polyethylene having a molecular weight of 40000 to 100000.
According to a preferred embodiment of the present invention, the diluent includes at least one of vegetable oil, liquid paraffin and diphenyl ether.
According to a preferred embodiment of the present invention, the vegetable oil comprises at least one of peanut oil, castor oil and soybean oil.
According to a preferred embodiment of the present invention, the nucleating agent comprises at least one of adipic acid, benzoic acid, pimelic acid and dibenzyl sorbitol.
According to a preferred embodiment of the invention, the temperature of the melting treatment is 175-230 ℃ and the time is 0.5-3h; the time of the defoaming treatment is 0.5-3h.
According to a preferred embodiment of the present invention, the step 1A may be performed as follows: adding polypropylene, polyethylene, diluent and nucleating agent into a spinning kettle with a stirring device to obtain a mixture, heating to 175-230 ℃, stirring for 0.5-3h under the condition of introducing nitrogen, and uniformly mixing; and after stirring is stopped, standing and defoaming for 0.5-3h to obtain the spinning solution.
According to some embodiments of the invention, the spinneret has a hole diameter of 0.1-5mm and a temperature of 140-180 ℃.
According to a preferred embodiment of the present invention, the step 1B may be performed as follows: filtering the spinning solution, then conveying the filtered spinning solution to a spinning nozzle by using a metering pump, and extruding the spinning solution through the spinning nozzle at a constant speed to obtain nascent fiber.
According to some embodiments of the invention, the nascent fiber is subjected to a cooling treatment in step S2 by passing through at least three stages of coagulation baths; preferably, the primary fiber is firstly cooled by staying in a primary coagulation bath at 100-120 ℃ for 5-20s, then cooled by staying in a secondary coagulation bath at 60-80 ℃ for 1-20s, and finally cooled by staying in a tertiary coagulation bath at 10-30 ℃ for 1-20s to prepare the fiber filament.
According to a preferred embodiment of the invention, the medium of the primary coagulation bath is a glycerol, polyethylene glycol or glyceryl triacetate solution with a mass concentration of 10-100%; and/or the medium of the secondary coagulation bath is deionized water; and/or the medium of the tertiary coagulation bath is deionized water. The coagulating bath and the diluent are dissolved and exchanged during the forming of the nascent fiber, so that the generation of a compact skin layer is avoided, and a large number of micropores can be generated on the surface of the fiber.
And after water bath treatment, winding and collecting the fiber filaments by using a traction wheel.
According to the invention, as-spun fibers are cooled and solidified by three different coagulation baths, the internal stress of the fibers can be reduced to the greatest extent, the phenomena of stress cracking, buckling deformation and the like are prevented, and the mechanical and thermal properties of the fibers are improved.
According to some embodiments of the invention, said step S3 comprises: placing the fiber filament into an extracting agent for extraction or placing the fiber filament into a plurality of extracting agents for sequential extraction; and/or the total extraction time is 3-48h.
According to a preferred embodiment of the present invention, the extractant comprises at least one of a ketone, an alcohol and an alkane, preferably at least one of acetone, methanol, isopropanol, n-hexane and cyclohexane, preferably at a concentration of more than 95%.
After extraction by the extractant, the diluent in the fiber filament can be separated and removed, so that pores are formed on the surface of the fiber, and the surface roughness and the surface area of the fiber are increased.
According to some embodiments of the invention, the method further comprises the steps of:
and S4, drying the prepared porous fiber for 12-24h, and removing the water on the surface to obtain the porous fiber.
According to another aspect of the present invention, there is also provided a porous fiber having a diameter of 0.1 to 5mm and a specific surface area of 19.0 to 29.5m, prepared according to the above method 2 /g。
According to another aspect of the invention, the application of the porous fiber in oil-water separation is also provided, which comprises the step of passing oily sewage through the porous fiber to separate an oil phase and a water phase in the oily sewage.
The porous fiber is an oleophilic material, when oily sewage passes through the porous fiber, oil drops in the sewage are coalesced on the surface of the fiber due to different affinities of an oil phase and a water phase to the fiber, so that the oil drops are changed from small to large, the oil drops after being changed in size float up due to smaller density, and further the separation of the oil phase and the water phase is realized.
According to another aspect of the present invention, there is also provided an apparatus for oil-water separation, including:
a liquid storage tank for storing oily sewage;
a coalescer connected to said tank and filled with said porous fiber for receiving and treating oily wastewater from said tank to separate oil and water phases therein;
a water production tank connected to said coalescer for receiving the aqueous phase from said coalescer;
an oil collection tank connected to the coalescer for receiving the oil phase from the coalescer.
According to some embodiments of the invention, the porous fibers are packed in a bed of the coalescer by layered compaction with a packing volume ratio of 1/2.
According to a preferred embodiment of the present invention, the coalescer is provided with a sewage inlet, a water phase outlet and an oil phase outlet. In some specific embodiments, the oil phase outlet is disposed in an upper portion of the coalescer, and the water phase outlet is disposed in a sidewall of the coalescer.
According to a preferred embodiment of the invention, the apparatus further comprises a sewage tank arranged between the liquid reservoir and the coalescer, the sewage tank being provided with a sewage inlet communicating with the liquid reservoir via a pipe, a sewage outlet communicating with the inlet of the coalescer via a pipe, and a gas inlet, for receiving sewage from the liquid reservoir and conveying it to the coalescer.
According to a preferred embodiment of the present invention, the apparatus further comprises a sewage pump disposed on the pipe between the tank and the sewage tank for pumping the sewage in the tank into the sewage tank.
According to a preferred embodiment of the invention, the apparatus further comprises a gas source connected to the gas inlet of the waste tank for supplying gas into the waste tank to propel waste into the coalescer. In some embodiments, the gas source is a nitrogen cylinder. The air source is connected with the sewage tank through a pipeline, and a pressure stabilizing valve is arranged on the pipeline.
According to a preferred embodiment of the present invention, the apparatus further comprises a flow regulating valve, a flow meter and a feed pump arranged in sequence on the pipe between the sewage tank and the coalescer.
According to a preferred embodiment of the invention, the water production tank communicates with the water phase outlet of the coalescer via a conduit, and the oil collection tank communicates with the oil phase outlet of the coalescer via a conduit.
The working process and the principle of the device for separating oil from water are as follows:
pumping oily sewage in the liquid storage tank into a sewage tank through a sewage pump, pumping liquid in the sewage tank into a coalescer through a feeding pump, and controlling the water inlet flow within 0.1-0.5m3/h by adjusting a flow regulating valve; the oil phase in the sewage is slowly attached to the surface of the porous fiber and then is gathered to form oil drops, the large-particle oil drops are carried away from the surface of the fiber by the water phase and enter the oil collecting tank through the oil phase outlet, and the water phase without the oil phase enters the water producing tank through the water phase outlet. Preferably, the temperature of the contaminated water is between 30 and 50 ℃.
According to another aspect of the invention, a method for oil-water separation by using the device is provided, which comprises the following steps:
(1) The porous fiber is compacted and filled into a bed layer of a coalescer in a layered mode, and the filling volume ratio is 1/2;
(2) Pumping the oily sewage with the temperature of 30-50 ℃ in the liquid storage tank into a sewage tank through a sewage pump;
(3) Opening a flow regulating valve, a flowmeter, a pressure stabilizing valve and an air source, pumping the liquid in the sewage tank into the coalescer by a feed pump, and controlling the inflow of water to be 0.1-0.5m by regulating the flow regulating valve 3 Within/h; the oil phase in the sewage is slowly attached to the surface of the fiber and then is gathered to form oil drops, the large-particle oil drops are carried away from the surface of the fiber by the water phase and enter the oil collecting tank through the oil phase outlet, and the water phase without the oil phase enters the water producing tank through the water phase outlet.
The invention has the advantages and beneficial technical effects as follows:
(1) The porous fiber material for oil-water separation is prepared by a thermally induced phase separation method, and the preparation process is simple and easy to operate;
(2) The main raw material polypropylene has rich sources, easily-controlled specification indexes and low price, has excellent chemical reagent resistance and higher mechanical strength, ensures that the quality of the prepared coalescent fiber is reliable, improves the mechanical property of the material by blending and adding high-density polyethylene, improves the lipophilic and hydrophilic balance, is beneficial to the flowing and falling of a surface oil film, and improves the coalescent and separation efficiency of oil drops in water;
(3) The primary fiber is dissolved and exchanged with the diluent during molding, so that a compact skin layer is avoided, a large number of micropores can be generated on the surface of the fiber, and the primary fiber is slowly cooled by the aid of the coagulating baths at different temperatures, so that internal stress of the fiber can be reduced to the maximum extent, mechanical and thermal properties of fiber coalescing materials are improved, and stress cracking, warping deformation and other phenomena are prevented;
(4) The addition of the nucleating agent improves the thermal stability, the impact strength and other properties of the prepared fiber, the pore size distribution is uniform, the pore-forming diluent and other additives are environment-friendly, non-toxic or low-toxic, the extracting agent is an industrial conventional reagent, and the second and third-stage coagulation baths are simple, convenient and easily-obtained non-solvent deionized water, so that the production cost in the whole process is greatly reduced;
(5) The oil-water separation equipment filled with the porous fiber has the advantages of compact structure, full sealing, safety, explosion prevention, realization of oil-sewage treatment device, high treatment efficiency, resource recycling of the recovered sewage oil, no waste residue generation and no secondary pollution.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus for oil-water separation according to the present invention;
description of reference numerals: 1: a gas source; 2: a liquid storage tank; 3: a pressure maintaining valve; 4: a sewage pump; 5: a sewage tank; 6: a flow regulating valve; 7: a flow meter; 8: a feed pump; 9: a coalescer; 10: a water production tank; 11: an oil collecting tank.
Detailed Description
The present invention is described below with reference to specific examples, which are not intended to limit the scope of the present invention, and those skilled in the art may make insubstantial modifications and adaptations of the present invention based on the above-described disclosure.
The starting materials used in the examples are all commercially available unless otherwise specified.
The test method comprises the following steps:
specific surface area test of the prepared fiber material is carried out according to national standard 'gas adsorption BET method determination solid matter specific surface area (GB/T19587-004'), and fiber diameter is determined by using XL-30 field emission scanning electron microscope.
The oil content in water is measured according to the national standard GB/T16488-1996 determination of water quality petroleum and animal and vegetable oil;
the oil removal rate was calculated as follows:
in the formula, C 0 Represents the oil content of the oily sewage in the sewage tank, mg/L;
c represents the oil content of the water phase in the water production tank, mg/L.
As shown in fig. 1, the apparatus for oil-water separation of the present invention comprises an air source 1, a liquid storage tank 2, a pressure-stabilizing valve 3, a sewage pump 4, a sewage tank 5, a flow-regulating valve 6, a flow meter 7, a feed pump 8, a coalescer 9, a water production tank 10, and a oil collection tank 11.
Wherein, the liquid storage tank 2 is used for storing oily sewage, the temperature of the sewage is 30-50 ℃, and the sewage is sequentially connected with a sewage pump 4 through a pipeline; the sewage pump 4 is connected to a sewage inlet of the sewage tank 5 through a pipe, and is used for pumping the oily sewage in the liquid storage tank 2 into the sewage tank 5. The gas source 1 is connected with a gas inlet of a sewage tank 5 through a pipeline, a pressure stabilizing valve 3 is arranged on the pipeline, and in the embodiment of the invention, the gas source 1 is preferably a nitrogen cylinder. The sewage outlet of the sewage tank 5 is connected with a feed pump 8 through a pipeline, a flow regulating valve 6 and a flow meter 7 are sequentially arranged on the pipeline, and the feed pump is connected with the inlet of a coalescer 9 through a pipeline and is used for pumping the sewage in the sewage tank 5 into the coalescer 9 for treatment. The coalescer 9 is filled with porous fibers to treat the wastewater and separate the oil phase from the water phase. The coalescer comprises an oil phase outlet and a water phase outlet, the oil phase outlet is connected with the oil collecting tank 11 through a pipeline, and the water phase outlet is connected with the water producing tank 10 through a pipeline.
Examples 1 to 24 and comparative examples 1 to 7
(1) Adding polypropylene resin into a spinning kettle with a stirring device, mixing the polypropylene resin with high-density polyethylene, a diluent and a nucleating agent in proportion, heating to a certain temperature for melting, stirring for a period of time under the condition of introducing nitrogen, stopping stirring, standing for a period of time for defoaming, and obtaining a spinning solution.
(2) And filtering the spinning solution by a filter screen, conveying the spinning solution to a spinning nozzle by a metering pump, extruding the spinning solution melt at a constant speed to form nascent fibers, cooling by a three-stage coagulating bath to obtain fiber filaments, and winding and collecting by a traction wheel.
(3) And (3) extracting the prepared nascent fiber in an extracting agent for a period of time, naturally drying in a fume hood, and removing water adsorbed on the surface to obtain the porous fiber.
The data of each step are shown in Table 1.
TABLE 1
Examples 25 to 52 and comparative examples 8 to 16
The device shown in figure 1 is adopted to treat oily wastewater of a certain refinery, the pH of the wastewater is 7.5, and the oil content is 1186mg/L.
(1) The porous fibers prepared in examples 1 to 24 and comparative examples 1 to 7 are respectively packed into a bed layer of a coalescer in a layered compaction mode, and the packing ratio is 1/2;
(2) Pumping the oily sewage with the temperature of 30-50 ℃ in the liquid storage tank into a sewage tank through a sewage pump;
(3) Opening a flow regulating valve, a flowmeter, a pressure stabilizing valve and an air source, pumping the liquid in the sewage tank into the coalescer by a feed pump, and controlling the inflow rate to be 0.1-0.5m by regulating the flow regulating valve 3 /h。
And measuring data after the operation is stable, and calculating to obtain the oil removal rate.
The data for each example and comparative example are shown in Table 2.
TABLE 2
Any numerical value mentioned in this specification, if there is only a two unit interval between any lowest value and any highest value, includes all values from the lowest value to the highest value incremented by one unit at a time. For example, if it is stated that the amount of a component, or a value of a process variable such as temperature, pressure, time, etc., is 50-90, it is meant in this specification that values of 51-89, 52-88, 69-71, and 70-71, etc., are specifically enumerated. For non-integer values, units of 0.1, 0.01, 0.001, or 0.0001 may be considered as appropriate. These are only some specifically named examples. In a similar manner, all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be disclosed in this application.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (11)
1. A preparation method of porous fiber for oil-water separation comprises the following steps:
s1, spinning a mixture containing polypropylene, polyethylene, a diluent and a nucleating agent to obtain nascent fiber; in the mixture, the mass percent of the polypropylene is 17-85.5%, the mass percent of the polyethylene is 1-13.5%, the mass percent of the nucleating agent is 0.1-5%, and the balance is the diluent;
s2, cooling the nascent fiber to obtain a fiber filament; in the step S2, the nascent fiber is cooled through at least three stages of coagulation baths; specifically, the nascent fiber is firstly cooled through a primary coagulation bath at 100-120 ℃, then cooled through a secondary coagulation bath at 60-80 ℃, and finally cooled through a tertiary bath at 10-30 ℃ to prepare the fiber filament;
and S3, extracting the fiber filaments to obtain the porous fiber for oil-water separation.
2. The method according to claim 1, wherein the step S1 includes:
1A, melting and defoaming a mixture containing polypropylene, polyethylene, a diluent and a nucleating agent to obtain a spinning solution;
and 1B, conveying the spinning solution to a spinning nozzle, and extruding through the spinning nozzle to obtain nascent fibers.
3. The method according to claim 1 or 2, wherein the temperature of the melt-processing is 175-230 ℃ and the time is 0.5-3h; the time of the defoaming treatment is 0.5-3h.
4. The method of claim 1 or 2, wherein the spinneret has a hole diameter of 0.1 to 5mm and a temperature of 140 to 180 ℃.
5. The preparation method according to claim 1 or 2, characterized in that the medium of the primary coagulation bath is a glycerol, polyethylene glycol or triacetin solution with a mass concentration of 10-100%; and/or the medium of the secondary coagulation bath is deionized water; and/or the medium of the tertiary coagulation bath is deionized water.
6. The method according to claim 1 or 2, wherein the step S3 includes: placing the fiber filament into an extracting agent for extraction or placing the fiber filament into a plurality of extracting agents for sequential extraction; and/or the total extraction time is 3-48h.
7. The method of claim 1 or 2, wherein the extractant comprises at least one of a ketone, an alcohol, and an alkane.
8. The method of claim 1, wherein the extractant comprises at least one of acetone, methanol, ethanol, isopropanol, n-hexane, and cyclohexane.
9. The porous fiber for oil-water separation prepared by the method according to any one of claims 1 to 8, which has a diameter of 0.1 to 5mm and a specific surface area of 19.0 to 29.5m 2 /g。
10. Use of the porous fiber for oil-water separation prepared by the method according to any one of claims 1 to 8 or the porous fiber for oil-water separation according to claim 9 in oil-water separation, comprising passing oily sewage through the porous fiber to separate an oil phase and a water phase therein.
11. An apparatus for oil-water separation, comprising:
a liquid storage tank for storing oily sewage;
a coalescer connected to the liquid tank and filled with the porous fiber prepared by the method according to any one of claims 1 to 8 or the porous fiber of claim 9 for receiving the oily wastewater from the liquid tank and treating the same to separate an oil phase and a water phase therein;
a water production tank connected to said coalescer for receiving the aqueous phase from said coalescer;
an oil collection tank connected to the coalescer for receiving the oil phase from the coalescer.
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| DE10040897B4 (en) * | 2000-08-18 | 2006-04-13 | TransMIT Gesellschaft für Technologietransfer mbH | Nanoscale porous fibers of polymeric materials |
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| CN103657439A (en) * | 2012-09-07 | 2014-03-26 | 中国石油化工股份有限公司 | Polypropylene hollow fiber separating membrane and preparation method thereof |
| CN103981635A (en) * | 2014-05-09 | 2014-08-13 | 浙江省纺织测试研究院 | Preparation method of porous fiber non-woven fabric |
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