CN112442750A - 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 PDF

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Publication number
CN112442750A
CN112442750A CN201910799196.8A CN201910799196A CN112442750A CN 112442750 A CN112442750 A CN 112442750A CN 201910799196 A CN201910799196 A CN 201910799196A CN 112442750 A CN112442750 A CN 112442750A
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oil
fiber
water
coalescer
sewage
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CN112442750B (en
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杨丽
王玉杰
焦旭阳
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent 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
    • D01F6/46Monocomponent 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/40Devices for separating or removing fatty or oily substances or similar floating material
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/06Chemical 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

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 nascent fibers; s2, enabling the nascent fiber to pass through an air spinning range of 10-100 mm; s3, cooling the nascent fiber obtained in the step S2 to obtain a fiber filament; and 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 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

Preparation method and application of fiber material for oil-water separation
Technical Field
The invention relates to a preparation method of a fiber material for oil-water separation, the fiber material prepared by the method, application of the fiber material in oil-water separation, and a device for oil-water separation, belonging to the technical field of water treatment.
Background
The oil-containing sewage is generated in the processes of oil exploitation, oil refining, petrochemical industry, oil storage and transportation and the like, the yield of the oil-containing sewage in China is extremely high, more than 30 hundred million tons of oil-containing sewage are generated every year in the oil field and oil refining industries, the oil-containing sewage is one of the industrial waste water which is difficult to treat at present, along with the environmental protection requirement and the gradual strictness of energy conservation and consumption reduction, the oil-containing concentration of the discharged sewage is less than 10ppm specified in the comprehensive sewage discharge standard (GB 8978 plus 1996) and the oil refining industry pollutant discharge standard, and higher requirements are provided for 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 separator has the advantages of low power consumption, high separation efficiency, large operation elasticity and the like, when oily sewage passes through the coalescence separator, 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 film, the liquid film of the liquid drops is gradually deformed and thinned in the liquid discharging process, the liquid film is broken when reaching a critical value, the two liquid drops are fused and grow up, the small oil drops are gradually aggregated into large oil drops, and along with the traction force of water flow, the large oil drops break away from the adsorption of the coalescence material to realize falling and enter an oil layer under the action of buoyancy to. The technical key of the coalescence method for removing oil is a coalescence material which can be divided into a porous material, a fiber material, a granular material and the like, wherein the fiber material can be made into a material with a smaller diameter and a larger surface area, and the coalescence material has obvious oil removing effect. 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.
The porous fiber material with microporous structure is prepared through TIPS process, which has the key points and difficulties of the selection of small molecular compound (diluent), low volatility and high heat stability, and needs low toxicity and less negative effect on health and environment. Dibutyl phthalate and dioctyl phthalate in phthalate esters and diphenyl ether-containing systems which are reported to be used have biological and microbial toxicity, can enter organisms through gastrointestinal tracts, respiratory tracts and skin absorption, are easy to influence labor environment to generate harm in the preparation process of porous fibers, and are limited by European Union REACH regulations, so that the requirements on environment-friendly green diluents or low-toxicity and low-harm solvents are more and more strong along with increasingly strict environmental protection laws.
Disclosure of Invention
The invention aims to provide a preparation method of a fiber material for oil-water separation according to the defects in the prior art, oleophylic resin is prepared into a fiber material with a coalesced surface by a Thermal Induced Phase Separation (TIPS) method, the roughness and the surface area of the surface are increased, the method is simple and convenient in process and short in production path, the fiber material prepared by the method is moderate in pore size, high in mechanical strength and excellent in separation performance, and is applied to oil-water separation, the separation effect is good, the invention also provides a device for oil-water separation, the structure is simple, the power consumption is low, no medicament is required to be added, the oil stain in sewage can be well removed, the pollution is low, and the device has a good application prospect in the field of oil-containing sewage treatment.
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 nascent fibers;
s2, enabling the nascent fiber to pass through an air spinning range of 10-100 mm;
s3, cooling the nascent fiber obtained in the step S2 to obtain a fiber filament;
and S4, extracting the fiber filaments to obtain the fiber material.
According to some embodiments of the invention, the step S1 includes:
1A, melting and defoaming a mixture containing polypropylene, polyvinylidene fluoride and a diluent 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 present invention, in the mixture, the polypropylene accounts for 18 to 89 mass percent, the polyvinylidene fluoride accounts for 0.2 to 9 mass percent, and the balance is the diluent.
According to a preferred embodiment of the present invention, the polypropylene resin has a melt index of 0.1-100g/10min, and the polypropylene resin has good flowability, processability and mechanical properties in the melt index range, wherein the melt index is measured at a temperature of 230 ℃ and a load weight of 2.16 kg.
According to a preferred embodiment of the invention, the diluent comprises at least one of a polyoxyethylene alkylamine, a fatty amide or a fatty alcohol amide.
According to a specific embodiment of the present invention, the polyoxyethylene alkylamine comprises (C)14-C18) Tallow bis (2-hydroxyethyl) amine, (C)12-C14) Hydrogenated tallow bis (2-hydroxyethyl) amine, (C)14-C18) Hydrogenated tallow ethoxy amine, (C)14-C18) At least one of bis (2-hydroxyethyl) amine, octadecyl bis (2-hydroxyethyl) amine, and hydrogenated tallow amine polyoxyethylene ether.
According to a particular embodiment of the invention, the fatty amide is preferably N, N-diethyl lauramide.
According to a particular embodiment of the invention, said fatty alcohol amide is preferably lauric acid diethanolamide.
According to the preferred embodiment of the invention, the temperature of the melting treatment is 175-230 ℃, and the time is 0.5-3 h; the time of the defoaming treatment is 0.5-3 h.
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 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 an aperture of 0.1 to 5mm and a temperature of 140 ℃.
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 as-spun fiber is subjected to a cooling treatment in step S3 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 80-100 ℃ for 5-20s, then cooled by staying in a secondary coagulation bath at 50-70 ℃ for 1-20s, and finally cooled by staying in a tertiary coagulation bath at 0-20 ℃ for 1-20s to prepare 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 content is between 0 and 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 tertiary coagulation bath is deionized water. The coagulation 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, the step S4 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 3-48 h.
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, ethanol, isopropanol, n-hexane and cyclohexane.
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:
s5, drying the prepared fiber material for 12-24h, 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 18.7-28.9m2/g。
According to another aspect of the present invention, there is also provided the use of the above fibrous material in oil-water separation, comprising passing oily wastewater through the fibrous material to separate an oil phase and an aqueous phase therein.
The fiber material is an oleophilic material, when 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, 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 fibrous material for receiving oily wastewater from said tank and treating the same 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 fibrous material is packed in layers compacted in the bed of the coalescer 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 liquid tank and the sewage tank, for pumping the sewage in the liquid 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 gas 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 by means of a conduit, and the oil collection tank communicates with the oil phase outlet of the coalescer by means of a conduit.
The working process and the principle of the device for oil-water separation 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 feeding pump, and controlling the inflow of water to be 0.1-0.5m by adjusting a flow regulating valve3Within/h; 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. The preferred temperature of the wastewater is 30-50 ℃.
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) compacting fibrous materials in layers and filling the fibrous materials into a bed layer of a coalescer, 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 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 valve3Within/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) according to the invention, the polypropylene coalescence fiber material with a porous surface and used for oil-water separation is obtained by adopting a simple process and adopting a green, environment-friendly and nontoxic diluent, a coagulating bath and an extracting agent, so that the roughness and the surface area of the surface structure of the fiber are increased, 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 oleophylic and hydrophilic 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 is improved.
(2) In the invention, the coagulation bath and the diluent are dissolved and exchanged during the molding of the nascent fiber, so that the generation of a compact skin layer is avoided, a large number of micropores can be generated on the surface of the fiber, and the nascent fiber is slowly cooled by the coagulation bath at different temperatures, so that the internal stress of the fiber can be reduced to the maximum extent, the mechanical and thermal properties of a fiber coalescence material are improved, and the phenomena of stress cracking, warping 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, the filled and prepared oil-water separation equipment has compact structure, full sealing, safety and explosion resistance, realizes the device treatment of oily sewage, has high treatment efficiency, can recycle the recovered dirty oil, does not generate any waste residue, and does not cause secondary pollution.
Drawings
FIG. 1 is a schematic structural diagram 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 producing 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:
the specific surface area of the prepared fiber material is measured according to national standard GB/T19587-.
The oil content in the water is measured according to the national standard GB/T16488 and 1996 determination of water quality petroleum and animal and vegetable oil;
the oil removal rate was calculated as follows:
Figure BDA0002181236960000071
in the formula, C0Represents 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 with a sewage inlet of the sewage tank 5 through a pipeline 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 fibrous material to treat the wastewater and separate the oil and water phases. 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 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 for defoaming, and obtaining a spinning solution.
(2) And after 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 fiber, performing air spinning, cooling by a three-stage coagulating bath to obtain fiber filament, and winding and collecting by a traction wheel.
(3) And (3) putting the prepared fiber filaments into an extracting agent for extracting for a period of time, then naturally drying in a fume hood, and removing the water adsorbed on the surface to prepare the fiber material.
The data of each step are shown in Table 1.
TABLE 1
Figure BDA0002181236960000091
Figure BDA0002181236960000101
Figure BDA0002181236960000111
Figure BDA0002181236960000121
Figure BDA0002181236960000131
Figure BDA0002181236960000141
Examples 29 to 59 and comparative examples 12 to 23
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 1479 mg/L.
(1) The fibrous materials prepared in examples 1-28 and comparative examples 1-11 were packed in layers in a coalescer bed at a packing volume ratio of 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 valve3/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
Figure BDA0002181236960000151
Figure BDA0002181236960000161
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 to 90, it is meant in this specification that values of 51 to 89, 52 to 88. 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 (12)

1. A method for preparing a fiber material for oil-water separation, comprising the following steps:
s1, spinning a mixture containing polypropylene, polyvinylidene fluoride and a diluent to obtain nascent fibers;
s2, enabling the nascent fiber to pass through an air spinning range of 10-100 mm;
s3, cooling the nascent fiber obtained in the step S2 to obtain a fiber filament;
and S4, extracting the fiber filaments to obtain the fiber material.
2. The method for preparing a composite material according to claim 1, wherein the step S1 includes:
1A, melting and defoaming a mixture containing polypropylene, polyvinylidene fluoride and a diluent 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 mixture comprises 18 to 89.1 mass% of polypropylene, 0.2 to 9 mass% of polyvinylidene fluoride, and the balance of diluent.
4. The method according to any one of claims 1 to 3, wherein the temperature of the melting treatment is 175-230 ℃ and the time is 0.5-3 h; the time of the defoaming treatment is 0.5-3 h.
5. The production method as claimed in any one of claims 1 to 4, wherein the spinneret has a hole diameter of 0.1 to 5mm and a temperature of 140 ℃ to 180 ℃.
6. The production method according to any one of claims 1 to 5, wherein the as-spun fiber is subjected to a cooling treatment by passing through at least three stages of coagulation baths in the step S3; preferably, the as-spun fiber is first cooled through a primary coagulation bath at 80-100 ℃, then through a secondary coagulation bath at 50-70 ℃, and finally through a tertiary bath at 0-20 ℃ to produce the fiber filament.
7. The method of any one of claims 1-6, wherein 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%; and/or the medium of the secondary coagulation bath is deionized water; and/or the medium of the tertiary coagulation bath is deionized water.
8. The production method according to any one of claims 1 to 7, wherein the step S4 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 3-48 h.
9. The method of any one of claims 1-8, wherein 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.
10. Fibrous material for oil-water separation prepared according to the process of any one of claims 1 to 9, having a diameter of 0.1 to 5mm and a specific surface area of 18.7 to 28.9m2/g。
11. Use of a fibrous material produced according to the process of any one of claims 1 to 9 or a fibrous material according to claim 10 in oil and water separation comprising passing oily water through the fibrous material to separate an oil phase and an aqueous phase therein.
12. An apparatus for oil-water separation, comprising:
a liquid storage tank for storing oily sewage;
a coalescer connected to the tank and filled with the fibrous material prepared by the method of any one of claims 1 to 9 or the fibrous material of claim 10 for receiving the oily wastewater from the tank and treating the same 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.
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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
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