CN112442752B - 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 PDFInfo
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- CN112442752B CN112442752B CN201910799907.1A CN201910799907A CN112442752B CN 112442752 B CN112442752 B CN 112442752B CN 201910799907 A CN201910799907 A CN 201910799907A CN 112442752 B CN112442752 B CN 112442752B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention discloses a preparation method of polypropylene fiber for oil-water separation and the polypropylene fiber prepared by the method, which 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 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 polypropylene fibers. The method has the advantages of simple process, short production path, moderate pore diameter, high mechanical strength and excellent separation performance of the polypropylene fiber prepared by the method, and 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 polypropylene fiber for oil-water separation, a polypropylene fiber material prepared by the method and application of the polypropylene fiber material in oil-water separation, and also relates to a device for oil-water separation, belonging to the technical field of water treatment.
Background
The source of the oily sewage is wide, and in the crude oil extraction and processing processes in the petrochemical industry, oil storage, oil tanker leakage, marine oil spill accidents and the like can generate more oily sewage, and if the oily sewage can not be effectively treated, huge losses and long-term harm can be caused to the health and the environment of economy and mankind. Existing oily sewage treatment technologies such as gravity separation, centrifugation, filtration, air floatation and the like have the defects of long existing time, large equipment volume, high equipment corrosion rate, large use of chemical agents and the like.
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 in the phthalate esters are reported to have biological micro toxicity, can enter the body through gastrointestinal tract, respiratory tract and skin absorption, are easy to influence the labor environment to generate harm in the porous fiber preparation process, and are limited to be used 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 the increasingly strict environmental protection laws.
Disclosure of Invention
According to the defects in the prior art, the invention provides a preparation method of polypropylene fibers for oil-water separation, which uses an environment-friendly nontoxic phthalate compound as a diluent and simultaneously adds a nucleating agent, and the lipophilic resin is prepared into fiber materials with coalesced surfaces through thermal phase separation, so that the roughness and the surface area of the surfaces are increased.
According to one 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 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 polypropylene fibers.
According to some embodiments of the invention, the step S1 includes:
1A, carrying out melting and defoaming treatment on a mixture containing polypropylene, a diluent and a nucleating agent 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 20-90% by mass, the nucleating agent is present in an amount of 0.1-5% by mass, and the remainder 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 a vegetable oil and optionally a phthalate compound, wherein the content of the vegetable oil in 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 present invention, the phthalate compound comprises dicyclohexyl phthalate and/or di (2-propylheptyl) phthalate.
According to a preferred embodiment of the present invention, the nucleating agent comprises a β -crystal form 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.
According to a preferred embodiment of the present invention, the amide-based nucleating agent comprises N, N-dicyclohexyl terephthalamide and/or N, N-dicyclohexyl terephthalamide-2, 6-naphthalene diamide.
According to a preferred embodiment of the present invention, the sorbitol nucleating agent comprises TMB-1 (tetramethylbenzidine); and/or the rare earth metal-based nucleating agent comprises at least one of WBG (a combination of rare earth metal oxide, rare earth metal stearate), calcium pimelate and calcium suberate.
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, a diluent and a 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 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 as-spun fibers are first cooled by a primary coagulation bath at 100-120 ℃, then by a secondary coagulation bath at 50-80 ℃, and finally by a tertiary coagulation bath at 0-20 ℃ to produce the fiber filaments.
According to a preferred embodiment of the invention, the medium of the primary coagulation bath comprises vegetable oil and optionally phthalate compounds, wherein the content of vegetable oil in the diluent is 10-100%; 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 three-stage coagulation bath is deionized water.
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, preferably the concentration of the extractant is more than 95%.
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 polypropylene fiber for 12-24 hours, and removing surface moisture to obtain the polypropylene fiber.
According to another aspect of the present invention, there is also provided a polypropylene fiber prepared according to the above method, having a diameter of 0.1 to 5mm and a specific surface area of 18.3 to 28.7m 2 /g。
According to another aspect of the invention, there is also provided the use of the polypropylene fiber as described above for oil-water separation, comprising passing oily wastewater through the polypropylene fiber, separating the oil phase from the water phase therein.
When the 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 an aqueous 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 small density, and further the separation of the oil phase and the aqueous 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 with the liquid storage tank, wherein the coalescer is filled with the polypropylene fibers and is used for receiving the oily sewage from the liquid storage tank and treating the oily sewage to separate an oil phase and a 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 polypropylene fibers are packed into the bed of the coalescer in a layered compacted manner at 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 polypropylene fiber, and then is 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. Preferably, the temperature of the wastewater 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) Layering, compacting and filling polypropylene fibers into a bed layer of a coalescer according to a filling 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 through a feed pump, and regulatingThrottle regulating valve to control water inflow rate of 0.1-0.5m 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:
the invention uses the diluent which does not contain dibutyl phthalate (DBP) or dioctyl phthalate (DOP), adds the nucleating agent, controls the types and the concentration of components of the coagulating bath, the coagulating bath temperature and the coagulating bath stage number, and prepares the polypropylene fiber material for treating the oily sewage, the surface of which has a large number of micropore structures, through a safe, environment-friendly and simple Thermal Induced Phase Separation (TIPS) method process. 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, a large number of micropores can be formed on the surface of the fiber, and the coagulating bath at different temperatures is slowly cooled, 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 polypropylene fiber coalescent material are improved, and the phenomena of stress cracking, buckling deformation and the like are prevented; the addition of the nucleating agent improves the thermal stability, impact strength and other performances of the prepared fiber, and the pore size distribution is uniform.
The polypropylene coalescent fiber material with the micropore structure is prepared by a simple process, the roughness and the surface area of the fiber surface structure are increased, oil drops are captured by the material and are converged and combined on the surface, the coalescence and oil-water separation efficiency is improved, and the filled oil-water separation equipment is compact in structure, fully closed, safe and explosion-proof, realizes the oil-containing sewage treatment device, has high treatment efficiency, can recycle recovered dirty oil, does not generate any waste residues, 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 polypropylene fibers to treat sewage and separate oil phase and 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 26 and comparative examples 1 to 11
(1) Adding polypropylene resin into a spinning kettle with a stirring device, mixing 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, 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 polypropylene fibers are prepared.
The data of each step are shown in Table 1.
The WBG used in the examples was purchased from guangdong bright linna new materials technologies inc.
TABLE 1
Examples 27 to 56 and comparative examples 12 to 23
The device shown in FIG. 1 is used for treating oily wastewater of a certain refining enterprise, and the pH value of the wastewater is 7.0, and the oil content is 1278mg/L.
(1) The polypropylene fibers prepared in examples 1-26 and comparative examples 1-11 were packed into the bed of the coalescer in a packing ratio of 1/2, respectively, by layer compaction;
(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 (13)
1. The preparation method of the 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; the aperture of the spinning nozzle used for the spinning treatment is 0.1-5mm; in the mixture, the mass percentage of polypropylene is 20-90%, the mass percentage of nucleating agent is 0.1-5%, and the rest is 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 cooling treatment comprises the steps of enabling the nascent fiber to pass through at least three-stage coagulating baths, firstly enabling the nascent fiber to pass through a primary coagulating bath at 100-120 ℃ for cooling, then pass through a secondary coagulating bath at 50-80 ℃ for cooling, and finally pass through a tertiary coagulating bath at 0-20 ℃ for cooling; the medium of the primary coagulation bath comprises vegetable oil and optional phthalate ester compounds, wherein the content of the vegetable oil is 10-100%; 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 S4, extracting the fiber filaments to obtain the polypropylene fiber for oil-water separation.
2. The method according to claim 1, wherein the step S1 comprises:
1A, carrying out melting and defoaming treatment on a mixture containing polypropylene, a diluent and a nucleating agent 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.
3. The preparation method according to claim 1 or 2, wherein the diluent comprises vegetable oil and optionally phthalate compound, wherein the content of vegetable oil in the diluent is 10-100%; 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.
4. The method of preparation of claim 1 or 2, wherein the nucleating agent comprises a β crystal form nucleating agent.
5. The method of claim 4, wherein the nucleating agent comprises at least one of an amide-based nucleating agent, a sorbitol-based nucleating agent, and a rare earth-based nucleating agent.
6. The process according to claim 5, wherein the amide-based nucleating agent comprises N, N-dicyclohexyl terephthalamide and/or N, N-dicyclohexyl terephthalamide; and/or the rare earth metal based nucleating agent is WBG.
7. The method according to claim 2, 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.
8. The method of claim 1 or 2, wherein the medium of the secondary coagulation bath is deionized water; and/or the medium of the three-stage coagulation bath is deionized water.
9. The preparation method according to claim 1 or 2, 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; and/or the extractant includes at least one of a ketone, an alcohol, and an alkane.
10. The method of claim 9, wherein the extractant comprises at least one of acetone, methanol, ethanol, isopropanol, n-hexane, and cyclohexane.
11. Polypropylene fiber for oil-water separation, prepared according to the method of any one of claims 1 to 10, having a diameter of 0.1 to 5mm and a specific surface area of 18.3 to 28.7m 2 /g。
12. Use of the polypropylene fiber prepared according to any one of claims 1 to 10 or the polypropylene fiber of claim 11 in oil-water separation, comprising passing oily water through the polypropylene fiber, separating an oil phase and an aqueous phase therein.
13. 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 polypropylene fibers prepared according to the method of any one of claims 1 to 10 or polypropylene fibers of claim 11 for receiving and treating oily wastewater from the tank to separate the oil phase and the water phase therein;
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.
Priority Applications (1)
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Citations (4)
| 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 |
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Patent Citations (4)
| 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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