CN112442752A - Preparation method and application of polypropylene fiber for oil-water separation - Google Patents

Preparation method and application of polypropylene fiber for oil-water separation Download PDF

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CN112442752A
CN112442752A CN201910799907.1A CN201910799907A CN112442752A CN 112442752 A CN112442752 A CN 112442752A CN 201910799907 A CN201910799907 A CN 201910799907A CN 112442752 A CN112442752 A CN 112442752A
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oil
fiber
polypropylene
nucleating agent
water
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CN112442752B (en
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杨丽
彭海珠
李宇
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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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • 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
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Removal Of Floating Material (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a preparation method of polypropylene fiber for oil-water separation and the polypropylene fiber prepared by the method, comprising the following steps: s1, spinning a mixture containing polypropylene, a diluent and a nucleating agent 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 polypropylene fibers. The method has simple and convenient process and short production path, and the polypropylene fiber prepared by the method has moderate aperture, high mechanical strength, excellent separation performance, high separation efficiency when being applied to oil-water separation. 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 polypropylene fiber for oil-water separation
Technical Field
The invention relates to a preparation method of polypropylene fiber for oil-water separation, a polypropylene fiber material prepared by the method, application of the polypropylene fiber material in oil-water separation, and a device for oil-water separation, belonging to the technical field of water treatment.
Background
The oily sewage has wide sources, and the crude oil extraction and processing processes, oil storage, oil tanker leakage, ocean oil spill accidents and the like in the petrochemical industry can generate more oily sewage, so that if the oily sewage cannot be effectively treated, the oily sewage can cause great loss and long-term harm to the economy, the human health and the environment. The existing oily sewage treatment technologies such as gravity separation, centrifugation, filtration, air floatation and the like have the defects of long time, large equipment volume, high equipment corrosion rate, use of a large amount of chemical agents and the like.
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 which are reported to be used have biological microbial toxicity, can enter organisms through gastrointestinal tracts, respiratory tracts and skin absorption, easily influence the working environment in the preparation process of porous fibers to cause harm, and are limited by the EU REACH regulation for use, so that the requirements on environment-friendly green diluents or low-toxic and low-harmful 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 polypropylene fiber for oil-water separation according to the defects in the prior art, which uses environment-friendly and nontoxic phthalate compounds as diluents, meanwhile, the nucleating agent is added, the oleophylic resin is prepared into the fiber material with the surface coalesced by a thermally induced phase separation method, the roughness and the surface area of the surface are increased, the method has simple and convenient process and short production path, the polypropylene fiber prepared by the method has moderate aperture, high mechanical strength and excellent separation performance, is applied to oil-water separation, the oil-water separation device has the advantages of simple structure, low power consumption, no need of adding any medicament, good effect of removing oil stains in sewage, low pollution and good application prospect in the field of oily sewage treatment.
According to an aspect of the present invention, there is provided a method for preparing polypropylene fibers for oil-water separation, comprising the steps of:
s1, spinning a mixture containing polypropylene, a diluent and a nucleating agent 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 polypropylene fibers.
According to some embodiments of the invention, the step S1 includes:
1A, melting and defoaming a mixture containing polypropylene, 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 a preferred embodiment of the present invention, in the mixture, the polypropylene accounts for 20 to 90 mass%, the nucleating agent accounts for 0.1 to 5 mass%, 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 present invention, the diluent comprises a vegetable oil and optionally a phthalate ester compound, wherein the vegetable oil content of the diluent is 10-100%.
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 invention, said phthalate-like compounds comprise dicyclohexyl phthalate and/or di (2-propylheptyl) phthalate.
According to a preferred embodiment of the present invention, the nucleating agent comprises a beta-crystalline nucleating agent, preferably at least one of an amide nucleating agent, a sorbitol nucleating agent and a rare earth metal nucleating agent.
According to a preferred embodiment of the present invention, the amide-based nucleating agent comprises N, N-dicyclohexylterephthalamide and/or N, N-dicyclohexyl-p-benzene-2, 6-naphthalenediamide.
According to a preferred embodiment of the present invention, the sorbitol-based nucleating agent comprises TMB-1 (tetramethylbenzidine); and/or the rare earth metal nucleating agent comprises at least one of WBG (complex of rare earth metal oxide and rare earth metal stearate), pimelic acid calcium salt and suberic acid calcium salt.
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, 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 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 as-spun fiber is first cooled through a primary coagulation bath at 100-120 ℃, then through a secondary coagulation bath at 50-80 ℃, and finally through a tertiary coagulation bath at 0-20 ℃ to produce the fiber filament.
According to a preferred embodiment of the invention, the medium of the primary coagulation bath comprises vegetable oil and optionally a phthalate compound, wherein the vegetable oil content of the diluent is between 10 and 100%; and/or the vegetable oil comprises at least one of peanut oil, castor oil, and soybean oil; and/or the phthalate compound comprises dicyclohexyl phthalate and/or di (2-propylheptyl) phthalate; and/or the medium of the secondary coagulation bath is deionized water; and/or the medium of the tertiary coagulation bath is deionized water.
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, 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:
s5, drying the prepared polypropylene fiber for 12-24h, and removing surface moisture to obtain the polypropylene fiber.
According to another aspect of the present invention, there is also provided a polypropylene fiber having a diameter of 0.1 to 5mm and a specific surface area of 18.3 to 28.7m prepared according to the above method2/g。
According to another aspect of the present invention, there is also provided a use of the polypropylene fiber described above in oil-water separation, comprising passing oily sewage through the polypropylene fiber to separate an oil phase and a water phase therein.
The polypropylene fiber is an oleophilic material, when oily sewage passes through the polypropylene 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 polypropylene fibers 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 polypropylene fibers are packed in a bed of the coalescer by layered compaction at 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 water inflow by adjusting a flow regulating valveThe flow rate is 0.1-0.5m3Within/h; the oil phase in the sewage is slowly attached to the surface of the polypropylene 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 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) the polypropylene fibers are compacted and filled into a bed layer of a coalescer layer in a layered mode, and the filling 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:
the invention uses a diluent without dibutyl phthalate (DBP) or dioctyl phthalate (DOP), adds a nucleating agent, controls the types and component concentrations of components of a coagulating bath, the temperature of the coagulating bath and the number of the coagulating bath stages, and prepares the polypropylene fiber material with a large number of microporous structures on the surface for treating oily sewage by a safe, environment-friendly and simple Thermal Induced Phase Separation (TIPS) method process. 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 and the like of a polypropylene fiber coalescence material are improved, and the phenomena of stress cracking, warping deformation and the like are prevented; the addition of the nucleating agent improves the thermal stability, the impact strength and other properties of the prepared fiber, and the pore size distribution is uniform.
The invention prepares the polypropylene coalescent fiber material with the micropore structure by a simple and convenient process, increases the roughness and the surface area of the fiber surface structure, is beneficial to capturing oil drops by the material and converging and combining the oil drops on the surface, improves the coalescent and oil-water separation efficiency, and the filled and prepared oil-water separation equipment has compact structure, full sealing, safety and explosion resistance, realizes the treatment of oily sewage, has high treatment efficiency, can recycle the recovered dirty oil, does not generate any waste residue, and can 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 BDA0002181535720000071
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 polypropylene fibers 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 26 and comparative examples 1 to 11
(1) Adding polypropylene resin into a spinning kettle with a stirring device, mixing the polypropylene resin with 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 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, naturally drying in a fume hood, and removing water adsorbed on the surface to prepare the polypropylene fiber.
The data of each step are shown in Table 1.
WBG used in the examples was purchased from Guangdong bright Linnan New materials science and technology, Inc.
TABLE 1
Figure BDA0002181535720000091
Figure BDA0002181535720000101
Figure BDA0002181535720000111
Figure BDA0002181535720000121
Figure BDA0002181535720000131
Figure BDA0002181535720000141
Figure BDA0002181535720000151
Examples 27 to 56 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 7.0, and the oil content of the wastewater is 1278 mg/L.
(1) The polypropylene fibers prepared in examples 1 to 26 and comparative examples 1 to 11 were packed in layers in a coalescer bed at a packing 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 BDA0002181535720000161
Figure BDA0002181535720000171
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 preparation method of polypropylene fiber for oil-water separation comprises the following steps:
s1, spinning a mixture containing polypropylene, a diluent and a nucleating agent 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 polypropylene fiber for oil-water separation.
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, 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 mixture comprises 20 to 90 mass% of the polypropylene, 0.1 to 5 mass% of the nucleating agent, and the balance of the diluent.
4. The method according to any one of claims 1 to 3, wherein the diluent comprises a vegetable oil and optionally a phthalate compound, wherein the vegetable oil content of the diluent is 10 to 100%; and/or the vegetable oil comprises at least one of peanut oil, castor oil, and soybean oil; and/or the phthalate compound comprises dicyclohexyl phthalate and/or di (2-propyl heptyl) phthalate.
5. The preparation method according to any one of claims 1 to 4, wherein the nucleating agent comprises a beta-crystalline nucleating agent, preferably at least one of an amide-based nucleating agent, a sorbitol-based nucleating agent and a rare earth metal-based nucleating agent; and/or the amide nucleating agent comprises N, N-dicyclohexyl terephthalamide and/or N, N-dicyclohexyl terephthalic-2, 6-naphthalene diamide; and/or the sorbitol nucleating agent comprises TMB-1; and/or the rare earth metal-based nucleating agent comprises at least one of WBG, calcium pimelate, and calcium suberate.
6. The method according to any one of claims 1 to 5, 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.
7. The production method according to any one of claims 1 to 6, wherein the as-spun fiber is subjected to a cooling treatment by passing through at least three stages of coagulation baths in step S3; preferably, the as-spun fiber is first cooled through a primary coagulation bath at 100-120 ℃, then through a secondary coagulation bath at 50-80 ℃, and finally through a tertiary coagulation bath at 0-20 ℃ to produce the fiber filament.
8. The method for preparing the high-temperature-resistant aqueous solution of any one of claims 1 to 7, wherein the medium of the primary coagulation bath comprises vegetable oil and optionally a phthalate compound, wherein the vegetable oil content in the diluent is 10 to 100%; and/or the vegetable oil comprises at least one of peanut oil, castor oil, and soybean oil; and/or the phthalate compound comprises dicyclohexyl phthalate and/or di (2-propylheptyl) phthalate; and/or the medium of the secondary coagulation bath is deionized water; and/or the medium of the tertiary coagulation bath is deionized water.
9. The method for preparing a porous material according to any one of claims 1 to 8, 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; and/or the extractant comprises at least one of ketone, alcohol and alkane, preferably at least one of acetone, methanol, ethanol, isopropanol, n-hexane and cyclohexane.
10. The polypropylene fiber for oil-water separation prepared by the method according to any one of claims 1 to 9, which has a diameter of 0.1 to 5mm and a specific surface area of 18.3 to 28.7m2/g。
11. Use of polypropylene fibers produced according to the process of any one of claims 1 to 9 or polypropylene fibers according to claim 10 for oil-water separation comprising passing oily water through said polypropylene fibers 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 liquid tank and filled with the polypropylene fiber produced by the method according to any one of claims 1 to 9 or the polypropylene fiber according to claim 10 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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Citations (4)

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Publication number Priority date Publication date Assignee Title
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
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
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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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