CN112442750B - Preparation method and application of fiber material for oil-water separation - Google Patents
Preparation method and application of fiber material for oil-water separation Download PDFInfo
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- CN112442750B CN112442750B CN201910799196.8A CN201910799196A CN112442750B CN 112442750 B CN112442750 B CN 112442750B CN 201910799196 A CN201910799196 A CN 201910799196A CN 112442750 B CN112442750 B CN 112442750B
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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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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- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a preparation method of a fiber material for oil-water separation and the fiber material prepared by the method, which comprises the following steps: s1, spinning a mixture containing polypropylene, polyvinylidene fluoride and a diluent to obtain a nascent fiber; s2, enabling the nascent fiber to pass through an air spinning process of 10-100 mm; s3, cooling the nascent fiber obtained in the step S2 to obtain a fiber filament; s4, extracting the fiber filaments to obtain the fiber material. The method has simple and convenient process and short production path, and the fiber material prepared by the method has moderate pore diameter, 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 consumption power, good removal effect on the greasy dirt in the sewage without adding any medicament, low pollution and good application prospect in the field of oily sewage treatment.
Description
Technical Field
The invention relates to a preparation method of a fiber material for oil-water separation, the fiber material prepared by the method and application thereof in oil-water separation, and also relates to a device for oil-water separation, belonging to the technical field of water treatment.
Background
The oil-containing sewage is produced in the processes of petroleum exploitation, petroleum refining, petrochemical industry, oil storage and transportation and the like, the output of the oil-containing sewage in China is extremely high, more than 30 hundred million tons of oil-containing sewage is produced in the oil field and oil refining industry each year, the oil-containing sewage is one of the industrial wastewater which is difficult to treat at present, and along with the gradual strictness of environmental protection requirements and energy conservation and consumption reduction, the oil concentration of the discharged sewage regulated in the comprehensive sewage discharge standard (GB 8978-1996) and the discharge standard of petroleum refining industrial pollutants is less than 10ppm, so that higher requirements are provided for the sewage treatment capacity and separation efficiency.
The coalescence-separation method is used as a physical oil removal method, integrates gravity separation and coalescence technology, and realizes the separation process by utilizing the characteristic of oil-water density difference. The coalescence separator has the advantages of low power consumption, high separation efficiency, high operation elasticity and the like, when oily sewage passes through the coalescence separator, oil drops interact with coalescence materials, and due to the lipophilicity of the material surface, the oil drops and the material surface form a continuous oil film with a certain thickness, when subsequent oil drops pass through the surface, liquid drops form a liquid clamping layer between the liquid drops and a layer film, the liquid film is gradually deformed and thinned in the liquid draining process, when the liquid film reaches a critical value, the liquid film is broken, the two liquid drops realize fusion and grow up, small oil drops gradually aggregate into large oil drops, and the large oil drops break off the adsorption of the coalescence materials along with the traction force of water flow, realize falling off, enter the oil layer and are separated under the action of floating force. The key technology of the coalescing method for removing oil is coalescing materials, wherein the coalescing materials can be divided into porous materials, fiber materials, granular materials and the like, and the fiber materials can be made into materials with smaller diameter and larger surface area, so that the coalescing method has remarkable oil removing efficiency. The agglomeration process mainly relies on interception and diffusion, only when oil drops move to the surface close to the material, the oil drops can be captured by the material under the action of Van der Waals attraction, so that the effect is only the outer surface, the larger the outer surface is, the higher the probability that the oil drops are close to the material and adhere to the material is, the more obvious influence is exerted on the agglomeration effect of the oil drops on the surface area of the material, the fiber material on the smooth surface can be increased by adopting a method of reducing the diameter, but the actual operation is extremely difficult due to the fact that the diameter of the agglomerated material is too small, so that the roughness of the surface of the material is desirably increased to achieve the aim of increasing the surface area.
The polymer porous fiber material with a microporous structure can be prepared by using a TIPS method, namely, a polymer and a high-boiling point small molecular compound (diluent) form a homogeneous solution at a high temperature (higher than the melting point of a crystalline polymer), solid-liquid or liquid-liquid phase separation can occur in the cooling process, and the porous fiber material with the microporous structure can be obtained after the diluent is removed. Dibutyl phthalate and dioctyl phthalate among the phthalates and diphenyl ether-containing systems which have been reported to be biologically micro-toxic and can be absorbed through gastrointestinal tract, respiratory tract and skin to enter the body, the labor environment is easily affected in the preparation process of the porous fiber to be harmful, and the use is limited by European Union REACH regulations, so that the requirements for environment-friendly green diluents or low-toxicity and low-toxicity solvents are becoming stronger as environmental protection laws are becoming stricter.
Disclosure of Invention
According to the defects existing in the prior art, the invention provides a preparation method of a fiber material for oil-water separation, which is characterized in that oleophilic resin is prepared into a fiber material with a coalesced surface by a Thermal Induced Phase Separation (TIPS) method, so that the surface roughness and the surface area are increased.
According to one aspect of the present invention, there is provided a method for preparing a fibrous material for oil-water separation, comprising the steps of:
s1, spinning a mixture containing polypropylene, polyvinylidene fluoride and a diluent to obtain a nascent fiber;
s2, enabling the nascent fiber to pass through an air spinning process of 10-100 mm;
s3, cooling the nascent fiber obtained in the step S2 to obtain a fiber filament;
s4, extracting the fiber filaments to obtain the fiber material.
According to some embodiments of the invention, the step S1 includes:
1A, carrying out melting and defoaming treatment on a mixture containing polypropylene, polyvinylidene fluoride and a diluent to obtain spinning solution;
and 1B, conveying the spinning solution to a spinneret, and extruding the spinning solution through the spinneret to obtain the primary fiber.
According to a preferred embodiment of the invention, in the mixture, the polypropylene is present in an amount of 18-89% by mass, the polyvinylidene fluoride is present in an amount of 0.2-9% by mass, and the balance is diluent.
According to the preferred embodiment of the invention, the melt index of the polypropylene resin is 0.1-100g/10min, the fluidity, the processing property and the mechanical property of the polypropylene resin raw material in the melt index range are good, 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 present invention, the diluent comprises at least one of polyoxyethylene alkylamine, fatty amide or fatty alcohol amide.
According to a specific embodiment of the present invention, the polyoxyethylene alkylamine comprises (C 14 -C 18 ) Tallow bis (2-hydroxyethyl) amine, (C) 12 -C 14 ) Hydrogenated tallow bis (2-hydroxyethyl) amine, (C) 14 -C 18 ) Hydrogenated tallow ethoxyamine, (C) 14 -C 18 ) At least one of bis (2-hydroxyethyl) amine, octadecyl bis (2-hydroxyethyl) amine, and hydrogenated tallow amine polyoxyethylene ether.
According to a specific embodiment of the invention, the fatty amide is preferably N, N-diethyllauramide.
According to a specific embodiment of the invention, the fatty alcohol amide is preferably lauric acid diethanolamide.
According to a preferred embodiment of the invention, the temperature of the melting treatment is 175-230 ℃ for 0.5-3 hours; 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, polyvinylidene fluoride and a diluent 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 stopping stirring, and standing for deaeration for 0.5-3h to obtain the spinning solution.
According to some embodiments of the invention, the spinneret has a pore size 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: and filtering the spinning solution, conveying the filtered spinning solution to a spinneret by using a metering pump, and extruding the spinning solution through the spinneret at a constant speed to obtain the nascent fiber.
According to some embodiments of the invention, in step S3, the nascent fiber is subjected to a cooling treatment by at least three stages of coagulation baths; preferably, the primary fiber is first cooled by a primary coagulation bath residence time of 80-100 ℃ for 5-20s, then by a secondary coagulation bath residence time of 50-70 ℃ for 1-20s, and finally by a tertiary coagulation bath residence time of 0-20 ℃ for 1-20s to produce the fiber filament.
According to a preferred embodiment of the invention, the medium of the primary coagulation bath comprises a diluent and optionally a vegetable oil, wherein the vegetable oil is present in an amount of 0-90%; the vegetable oil is preferably soybean oil, castor oil, corn oil or peanut oil; and/or the medium of the secondary coagulation bath is deionized water; and/or the medium of the three-stage coagulation bath is deionized water. The coagulating bath and the diluent are dissolved and exchanged when the nascent fiber is formed, so that the formation of a compact cortex is avoided, and a large number of micropores can be formed on the surface of the fiber.
After the water bath treatment, the fiber filaments are wound and collected by a traction wheel.
The invention can furthest reduce the internal stress of the fiber, prevent the phenomena of stress cracking, buckling deformation and the like and improve the mechanical property, the thermal property and the like of the fiber by cooling and solidifying the nascent fiber through three-stage different coagulating baths.
According to some embodiments of the invention, the step S4 includes: extracting the fiber filaments in one extractant or extracting the fiber filaments in a plurality of extractants in sequence; and/or, the total extraction time is 3-48h.
According to a preferred embodiment of the invention, the extractant comprises at least one of a ketone, an alcohol and an alkane, preferably at least one of acetone, methanol, ethanol, isopropanol, n-hexane and cyclohexane.
After extraction by the extractant, the diluent in the fiber filaments can be separated and removed, so that pores are formed on the surface of the fibers, and the surface roughness and the surface area of the fibers are increased.
According to some embodiments of the invention, the method further comprises the steps of:
s5, drying the prepared fiber material for 12-24 hours, and removing surface moisture to obtain the fiber material.
According to another aspect of the present invention, there is also provided a fibrous material prepared according to the above method, having a diameter of 0.1 to 5mm and a specific surface area of 18.7 to 28.9m 2 /g。
According to another aspect of the invention, there is also provided the use of the above-mentioned fibrous material in oil-water separation, comprising passing oily sewage through the fibrous material, separating the oil phase and the water phase therein.
When the oily sewage passes through the fiber material, oil drops in the sewage are coalesced on the surface of the fiber due to different affinities of the oil phase and the water phase to the fiber, so that the oil drops are changed from small to large, and the changed oil drops float upwards due to the 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, comprising:
the liquid storage tank is used for storing oily sewage;
a coalescer connected to the tank and filled with the fibrous material for receiving and treating the oily wastewater from the tank to separate the oil phase from the water phase;
a water producing tank connected to the coalescer for receiving the aqueous phase from the coalescer;
and the oil collecting tank is connected with the coalescer and is used for receiving the oil phase from the coalescer.
According to some embodiments of the invention, the fibrous material is packed into the bed of the coalescer in a layered compaction with a packing volume ratio of 1/2.
According to a preferred embodiment of the invention, the coalescer is provided with a sewage inlet, an aqueous 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 aqueous phase outlet is disposed in a sidewall of the coalescer.
According to a preferred embodiment of the invention, the device further comprises a sewage tank arranged between the liquid storage tank and the coalescer, the sewage tank being provided with a sewage inlet, a sewage outlet and a gas inlet, the sewage inlet of which is in communication with the liquid storage tank via a pipe, and the sewage outlet of which is in communication with the inlet of the coalescer via a pipe for receiving sewage from the liquid storage tank and for conveying to the coalescer.
According to a preferred embodiment of the invention, the device further comprises a sewage pump arranged on the pipeline between the liquid storage tank and the sewage tank for pumping the sewage in the liquid storage tank into the sewage tank.
According to a preferred embodiment of the invention, the device further comprises a gas source connected to the gas inlet of the sewage tank for feeding gas into the sewage tank for pushing sewage into the coalescer. In some specific 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 invention, the device further comprises a flow regulating valve, a flow meter and a feed pump arranged in sequence on the conduit between the sewage tank and the coalescer.
According to a preferred embodiment of the invention, the water-producing tank communicates with the water phase outlet of the coalescer by means of a pipe, and the oil-collecting tank communicates with the oil phase outlet of the coalescer by means of a pipe.
The working process and principle of the device for oil-water separation of the invention are as follows:
pumping oily sewage in a liquid storage tank into a sewage tank through a sewage pump, pumping liquid in the sewage tank into a coalescer through a feed pump, and controlling the flow of water inflow to be 0.1-0.5m by adjusting a flow regulating valve 3 Within/h; the oil phase in the sewage is slowly adhered to the surface of the porous fiber, so that oil drops are formed by aggregation, large-particle oil drops are carried by the water phase to leave the surface of the fiber, enter the oil collecting tank through the oil phase outlet, and enter the water producing tank through the water phase outlet after the oil phase is removed. Preferably, the sewage temperature is 30-50 ℃.
According to another aspect of the present invention, there is provided a method for oil-water separation using the above apparatus, comprising:
(1) Filling fibrous materials into a bed layer of a coalescer in a layering compaction manner, wherein 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 liquid in a sewage tank into a coalescer through a feed pump, and controlling the inflow water flow to be 0.1-0.5m by regulating the flow regulating valve 3 Within/h; the oil phase in the sewage is slowly adhered to the surface of the fiber so as to be aggregated to form oil drops, the large-particle oil drops are carried by the water phase to leave the surface of the fiber, enter the oil collecting tank through the oil phase outlet, and the water phase with the oil phase removed enters the water producing tank through the water phase outlet.
The invention has the following advantages and beneficial technical effects:
(1) According to the invention, the polypropylene coalescent fiber material with porous surface and used for oil-water separation is obtained by a simple process and by adopting the environment-friendly nontoxic diluent, the coagulating bath and the extractant, the roughness and the surface area of the fiber surface structure are increased, the oil drops are favorably captured by the material and are converged and combined on the surface, and the coalescence and oil-water separation efficiency is improved; meanwhile, the hydrophilic-lipophilic balance of the prepared fiber material is improved by blending and adding polyvinylidene fluoride, so that the flow and the falling of a surface oil film are facilitated, and the coalescence and separation efficiency of oil drops in water are improved.
(2) According to the invention, the coagulating bath and the diluent are dissolved and exchanged during molding of the nascent fiber, so that the generation of a compact cortex is avoided, a large number of micropores can be generated on the surface of the fiber, and the coagulating bath at different temperatures is subjected to slow cooling, so that the internal stress of the fiber can be reduced to the greatest extent, the mechanical property, the thermal property and the like of the fiber coalescent material are improved, and the phenomena of stress cracking, buckling deformation and the like are prevented;
(3) The coalescent fiber material prepared by the invention has low price, excellent chemical reagent resistance and higher mechanical strength, and the filled oil-water separation equipment has compact structure, is totally closed, safe and explosion-proof, realizes oily sewage treatment device, has high treatment efficiency, can recycle recovered dirty oil, does not generate any waste residue and does not cause secondary pollution.
Drawings
FIG. 1 is a schematic diagram of a device for oil-water separation according to the present invention;
reference numerals illustrate: 1: a gas source; 2: a liquid storage tank; 3: a pressure stabilizing 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 producing tank; 11: 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, but rather, those skilled in the art can make various insubstantial improvements and modifications in light of the above teachings.
Unless otherwise indicated, all the starting materials used in the examples were commercially available.
The testing method comprises the following steps:
the specific surface area test of the prepared fiber material is carried out according to the national standard of measuring the specific surface area of solid substances (GB/T19587-004) by a gas adsorption BET method, and the fiber diameter is measured by utilizing an XL-30 field emission scanning electron microscope.
The oil content in water is measured according to the national standard GB/T16488-1996 determination of oil quality and animal and vegetable oil;
the oil removal rate is calculated as follows:
wherein C is 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 producing tank and mg/L.
As shown in fig. 1, the device for oil-water separation of the present invention comprises a gas 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 producing tank 10 and a collecting 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 connected with the sewage pump 4 in sequence through a pipeline; the sewage pump 4 is used for pumping the oily sewage in the liquid storage tank 2 into the sewage tank 5 through a pipeline and a sewage inlet of the sewage tank 5. The gas source 1 is connected to the gas inlet of the sewage tank 5 by a pipe on which a pressure stabilizing valve 3 is provided, 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 feeding pump 8 through a pipeline, a flow regulating valve 6 and a flowmeter 7 are sequentially arranged on the pipeline, and the feeding 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 fibrous material to treat the sewage and separate the oil phase from the water phase. The coalescer comprises an oil phase outlet and a water phase outlet, wherein 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 28 and comparative examples 1 to 11
(1) Adding polypropylene resin into a spinning kettle with a stirring device, mixing with polyvinylidene fluoride and a diluent 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, and defoaming to obtain spinning solution.
(2) After the spinning solution is filtered by a filter screen, the spinning solution is conveyed to a spinneret by a metering pump, then the spinning solution melt is extruded at a constant speed to form primary fibers, the primary fibers are subjected to an air spinning process and then are cooled by a three-stage coagulating bath, so that fiber filaments are obtained, and then the fiber filaments are wound and collected by a traction wheel.
(3) The prepared fiber filaments are put into an extractant for extraction for a period of time, then are naturally dried in a fume hood, and the moisture adsorbed on the surface is removed, so that the fiber material is prepared.
The data of each step are shown in Table 1.
TABLE 1
Examples 29 to 59 and comparative examples 12 to 23
The oily wastewater of a refinery is treated by the device shown in FIG. 1, and the oily content of the wastewater is 1479mg/L at pH 7.5.
(1) The fibrous materials prepared in examples 1-28 and comparative examples 1-11 were packed into the bed of the coalescer in a 1/2 packing volume ratio;
(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 liquid in a sewage tank into a coalescer through a feed pump, and controlling the inflow water flow to be 0.1-0.5m by regulating the flow regulating valve 3 /h。
And measuring data after running is stable, and calculating to obtain the oil removal rate.
The data of each example and comparative example are shown in Table 2.
TABLE 2
Any numerical value recited in this disclosure includes all values incremented by one unit from the lowest value to the highest value if there is only a two unit interval between any lowest value and any highest value. For example, if the amount of one component, or the value of a process variable such as temperature, pressure, time, etc., is stated to be 50-90, it means that values of 51-89, 52-88, and 69-71, and 70-71 are specifically recited in this specification. For non-integer values, 0.1, 0.01, 0.001 or 0.0001 units may be considered as appropriate. This is only a few examples of the specific designations. 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-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
Claims (16)
1. A method of preparing a fibrous material for oil-water separation comprising the steps of:
s1, spinning a mixture containing polypropylene, polyvinylidene fluoride and a diluent to obtain a nascent fiber; 1A, performing melting and defoaming treatment on a mixture containing polypropylene, polyvinylidene fluoride and a diluent to obtain spinning solution; 1B, conveying the spinning solution to a spinneret, and extruding the spinning solution through the spinneret to obtain nascent fibers; the aperture of the spinneret is 0.1-5mm; in the mixture, the polypropylene accounts for 18-89.1 percent by mass, the polyvinylidene fluoride accounts for 0.2-9 percent by mass, and the rest is the diluent;
s2, enabling the nascent fiber to pass through an air spinning process of 10-100 mm;
s3, cooling the nascent fiber obtained in the step S2 to obtain a fiber filament; the primary fiber is subjected to cooling treatment through at least three-stage coagulating baths, so that the primary fiber is firstly cooled through a primary coagulating bath at 80-100 ℃, then cooled through a secondary coagulating bath at 50-70 ℃, finally cooled through a tertiary bath at 0-20 ℃, wherein the medium of the primary coagulating bath comprises a diluent and optionally vegetable oil, the content of the vegetable oil is 0-90%, the medium of the secondary coagulating bath is deionized water, and the medium of the tertiary coagulating bath is deionized water;
and S4, extracting the fiber filaments to obtain the fiber material.
2. The method according to claim 1, wherein the melting treatment is carried out at a temperature of 175-230 ℃ for a time of 0.5-3 hours; the time of the defoaming treatment is 0.5-3h.
3. The method of claim 1, wherein the dope extrusion temperature is 140-180 ℃.
4. The method according to claim 1, wherein the step S4 comprises: extracting the fiber filaments in one extractant or extracting the fiber filaments in a plurality of extractants in sequence; and/or, the total extraction time is 3-48h.
5. The method of claim 4, wherein the extractant comprises at least one of a ketone, an alcohol, and an alkane.
6. The method according to claim 5, wherein the extractant comprises at least one of acetone, methanol, ethanol, isopropanol, n-hexane, and cyclohexane.
7. A fibrous material for oil-water separation prepared according to the method of any one of claims 1 to 6, having a diameter of 0.1 to 5mm and a specific surface area of 18.7 to 28.9m 2 /g。
8. Use of a fibrous material prepared according to the method of any one of claims 1-6 or a fibrous material of claim 7 in oil-water separation comprising passing oily wastewater through the fibrous material to separate the oil phase and the water phase therein.
9. An apparatus for oil-water separation comprising:
the liquid storage tank is used for storing oily sewage;
a coalescer connected to the tank filled with fibrous material prepared according to the method of any one of claims 1-6 or fibrous material of claim 7 for receiving and treating oily wastewater from the tank to separate the oil and water phases therein; the fiber materials are compacted and filled into a bed layer of the coalescer in a layering manner, and the filling volume ratio is 1/2;
a water producing tank connected to the coalescer for receiving the aqueous phase from the coalescer;
and the oil collecting tank is connected with the coalescer and is used for receiving the oil phase from the coalescer.
10. The apparatus of claim 9, wherein the coalescer is provided with a sewage inlet, a water phase outlet, and an oil phase outlet; the oil phase outlet is arranged at the upper part of the coalescer, and the water phase outlet is arranged at the side wall of the coalescer.
11. The apparatus of claim 9, further comprising a sewage tank disposed between the liquid storage tank and the coalescer, the sewage tank having a sewage inlet in communication with the liquid storage tank via a conduit, a sewage outlet in communication with the coalescer inlet via a conduit, and a gas inlet for receiving sewage from the liquid storage tank and delivering the sewage to the coalescer.
12. The apparatus of claim 11, further comprising a sewage pump disposed on a conduit between the tank and the tank for pumping sewage from the tank into the tank.
13. The apparatus of claim 11, further comprising a gas source connected to the gas inlet of the wastewater tank for inputting gas into the wastewater tank to push wastewater into the coalescer; the air 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.
14. The apparatus of claim 11, further comprising a flow regulating valve, a flow meter, and a feed pump disposed in sequence on a conduit between the wastewater tank and the coalescer.
15. The apparatus of claim 9, wherein the water-producing tank is in communication with the water phase outlet of the coalescer by a conduit and the oil-collecting tank is in communication with the oil phase outlet of the coalescer by a conduit.
16. The apparatus of claim 9, wherein the method for oil-water separation using the apparatus comprises:
(1) Filling fibrous materials into a bed layer of a coalescer in a layering compaction manner, wherein 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 liquid in a sewage tank into a coalescer through a feed pump, and controlling the inflow water flow to be 0.1-0.5m by regulating the flow regulating valve 3 Within/h; the oil phase in the sewage is slowly adhered to the surface of the fiber so as to be aggregated to form oil drops, the large-particle oil drops are carried by the water phase to leave the surface of the fiber, enter the oil collecting tank through the oil phase outlet, and the water phase with the oil phase removed enters the water producing tank through the water phase outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910799196.8A CN112442750B (en) | 2019-08-27 | 2019-08-27 | Preparation method and application of fiber material for oil-water separation |
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| CN103007784A (en) * | 2011-09-22 | 2013-04-03 | 中国石油化工股份有限公司 | Improved preparation method of polypropylene hollow fiber separation membrane |
| 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 |
| CN107385558A (en) * | 2017-08-10 | 2017-11-24 | 吉林省华纺静电材料科技有限公司 | A kind of multi-functional polypropene staple and its production technology |
| CN107540105A (en) * | 2016-06-28 | 2018-01-05 | 宝山钢铁股份有限公司 | A kind of deoiling method and its device of the dense oil emulsion waste water of cold rolling |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103007784A (en) * | 2011-09-22 | 2013-04-03 | 中国石油化工股份有限公司 | Improved preparation method of polypropylene hollow fiber separation membrane |
| 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 |
| CN107540105A (en) * | 2016-06-28 | 2018-01-05 | 宝山钢铁股份有限公司 | A kind of deoiling method and its device of the dense oil emulsion waste water of cold rolling |
| CN107385558A (en) * | 2017-08-10 | 2017-11-24 | 吉林省华纺静电材料科技有限公司 | A kind of multi-functional polypropene staple and its production technology |
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