CN115722209A - Polyoxymethylene microfiber oil-water separation material and preparation method thereof - Google Patents
Polyoxymethylene microfiber oil-water separation material and preparation method thereof Download PDFInfo
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- 229920006324 polyoxymethylene Polymers 0.000 title claims abstract description 173
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 229920001410 Microfiber Polymers 0.000 title claims abstract description 90
- 239000003658 microfiber Substances 0.000 title claims abstract description 90
- 238000000926 separation method Methods 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229930040373 Paraformaldehyde Natural products 0.000 title claims description 64
- -1 Polyoxymethylene Polymers 0.000 title claims description 64
- 239000000835 fiber Substances 0.000 claims abstract description 77
- 238000010008 shearing Methods 0.000 claims abstract description 27
- 238000009987 spinning Methods 0.000 claims abstract description 26
- 238000001179 sorption measurement Methods 0.000 claims abstract description 21
- 229920006240 drawn fiber Polymers 0.000 claims abstract description 19
- 238000000967 suction filtration Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000008187 granular material Substances 0.000 claims abstract description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 68
- 238000004804 winding Methods 0.000 claims description 44
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 22
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 238000002074 melt spinning Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims 1
- 238000000643 oven drying Methods 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 46
- 230000008018 melting Effects 0.000 abstract description 10
- 238000002844 melting Methods 0.000 abstract description 10
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- 239000010408 film Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
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- 239000003960 organic solvent Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
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- 230000000052 comparative effect Effects 0.000 description 4
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 238000005229 chemical vapour deposition Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
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Abstract
The invention provides a polyformaldehyde microfiber oil-water separation material and a preparation method thereof, and the preparation method comprises the following steps: polyformaldehyde nascent fibers are obtained by melting and spinning polyformaldehyde granules, and polyformaldehyde drawn fibers are obtained by hot drawing, so that a fibrillating structure is formed in the polyformaldehyde drawn fibers and the polyformaldehyde drawn fibers are orderly arranged along the axial direction. And (2) chopping polyformaldehyde stretched fibers, putting the chopped polyformaldehyde stretched fibers and water into a mechanical crusher, shearing, disassembling and crushing to obtain a polyformaldehyde microfiber water dispersion, performing suction filtration by using a suction bottle, and washing with deionized water and drying in an oven to obtain the polyformaldehyde microfiber oil-water separation material. The process is simple and convenient, and no chemical reagent is used in the preparation process, so that the environment is not polluted; the polyformaldehyde has chemical stability, plasticity and self-supporting property, has good adsorption and separation effects on various oils and organic reagents, can meet various oil-water separation environments and conditions, and provides an effective solution for treating offshore crude oil leakage and purifying oily sewage.
Description
The technical field is as follows:
the invention belongs to the field of novel material processing and preparation, relates to a preparation method of an oil-water separation material, and particularly relates to a polyformaldehyde microfiber oil-water separation material and a preparation method thereof.
Background
Recently, the treatment of offshore crude oil leakage and the purification of oily domestic sewage face more and more challenges, and the current treatment methods are roughly divided into the following methods: the oil on the water surface is recovered by using a hydrophobic and oleophilic material, the oil and the water are mixed by using a dispersing agent to promote natural degradation, and the oil and the water are directly combusted to remove floating oil. A generally preferred method is to recover the oil slick on the water surface by using a material having hydrophobic and oleophilic properties, which can properly treat the oil slick without causing secondary pollution. These hydrophobic and oleophilic materials currently used can be classified into hydrophobic powder materials, hydrophobic thin film materials, and hydrophobic three-dimensional porous materials. The sustao project group utilizes a chemical reaction method to thermally reduce an aqueous dispersion of graphite oxide to form graphene hydrogel, and then the graphene hydrogel is subjected to freeze drying to obtain graphene aerogel, and the prepared aerogel has a porous structure and hydrophobic oleophylic characteristics. The Wu Dehai subject group of Qinghua university prepares a three-dimensional porous spongy carbon nanotube fast-assembly material by a chemical vapor deposition method, and the carbon nanotube sponge has super-hydrophobic characteristics, rich void structures and super-light density, so that the material has stronger oil absorption capacity and can absorb organic solvents or oil products, but the preparation method is complex and has high cost. Meanwhile, when the oil-water separation material is prepared by the electrostatic spinning method commonly used in the prior art, the addition of an organic solvent is needed, the human health is harmed, the environment is polluted, the preparation time is long, the production efficiency is reduced, and the large-scale industrial production application is not facilitated. The preparation method has the characteristics of complex preparation process, environmental pollution caused by using chemical reagents and difficulty in large-scale production and application, and is not beneficial to guiding industrial production.
When the hydrophobic powder material is applied to the oil-water separation process, the material has larger oil absorption capacity due to the abundant space structure which can provide the space for storing oil products. The polyformaldehyde is one of wide general plastics, is cheap and easy to obtain, has stable chemical performance and hydrophobic and oleophilic properties, can be more effectively subjected to oil-water separation after being processed into a microfiber powder material, is easy to process and form, has low preparation cost, can be repeatedly utilized, and has remarkable advantages, important values and profound significance in actual large-scale continuous production and industrial application.
Disclosure of Invention
The invention aims to prepare the microfiber oil-water separation material which has the advantages of simple process flow, no addition of chemical reagents, no pollution, environmental friendliness, low cost, obvious oil adsorption and oil-water separation effects, chemical stability, recycling property and plasticity and capability of large-scale continuous production, and is simple and convenient to operate.
In order to achieve the purpose, the invention provides a preparation scheme of a polyoxymethylene microfiber oil-water separation material, which comprises the following steps:
(1) Adding the polyformaldehyde granules into a screw extruder of spinning equipment for spinning, obtaining polyformaldehyde nascent fibers without stretching multiplying power through melt spinning, then drafting the polyformaldehyde nascent fibers in an air drafting machine, and obtaining polyformaldehyde stretched fibers after winding through a winding machine;
(2) Chopping the polyformaldehyde stretched fibers obtained in the step (1) by using a cutter to obtain polyformaldehyde chopped fibers, putting the polyformaldehyde chopped fibers into a mechanical crusher, adding water, performing mechanical shearing crushing, and disassembling to obtain a polyformaldehyde microfiber water dispersion;
(3) And (3) carrying out suction filtration on the polyformaldehyde microfiber water dispersion obtained in the step (2), washing with deionized water, and then putting into an oven for drying to finally obtain the polyformaldehyde microfiber oil-water separation material.
Preferably, in the spinning process in the step (1), the temperatures of 6 zones of the single screw of the spinning machine are respectively 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, the rotating speed of the single screw of the extruder is 90rpm, the rotating speed of the metering pump is 60rpm, the winding speed of the winding machine is 300rpm, and the frequency of the reciprocating shaft is 200Hz.
Preferably, in the hot-drawing step of step (1), the temperature of 3 zones of hot-drawing is 100 ℃,110 ℃,120 ℃ and the draw ratio is 5 to 10 times. More preferably, the stretch ratio is 6 to 9 times, and most preferably 7 times.
Preferably, when the polyoxymethylene chopped fibers are mechanically sheared, crushed and disassembled in the step (2), 2 liters of water is added into the mechanical crusher at each time of shearing, crushing and disassembling, and the shearing rate is 10 5 s -1 The time is 5 to 120 minutes. More preferably 30 to 60 minutes, and most preferably 50 minutes.
Compared with the prior art, the invention has the following positive and beneficial effects:
(1) The invention utilizes the phenomenon that during the hot drawing process, fibrillated microfiber structures are generated inside fibers and are aligned along the axial direction of the fibers, and the anisotropic primary fibers of the drawn fibers do not exist, which can be proved by an XRD spectrogram (figure 3). The polyformaldehyde microfiber oil-water separation material is obtained by mechanically shearing, crushing and disassembling polyformaldehyde drawn fibers, destroying weak bonding force between radial directions of the microfibers, keeping strong bonding force (chemical bond) inside the microfibers, and enabling the polyformaldehyde microfibers to be mutually overlapped, interpenetrated and supported in a suction filtration mode (figure 2). The method for preparing the microfiber by mechanical shearing, crushing and disassembling solves the problem that the porous oil-water separation material is difficult to produce continuously, massively and at low cost in the existing preparation method, and greatly reduces the production cost.
(2) In the method for preparing the polyformaldehyde microfiber oil-water separation material, the used raw materials are cheap and easily available, and the polyformaldehyde microfiber oil-water separation material has excellent hydrophobicity, lipophilicity and chemical stability; the preparation process does not add chemical reagents, only uses deionized water, has no pollution to the environment, and is safe and environment-friendly in the processing process.
(3) The polyformaldehyde microfiber oil-water separation material prepared by the invention has micron-level holes formed by mutually inserting, overlapping and supporting a large number of microfibers, and has high air and oil-water contact angles, oil adsorption capacity and oil-water separation efficiency on various oils and organic solvents.
(4) As shown in FIG. 9, the polyoxymethylene microfiber material prepared by the invention is powdery, has plasticity, can be molded into various shapes, and can be molded into a self-supporting polyoxymethylene microfiber oil-water separation cup, so as to meet oil-water separation environments under various conditions, and provide a feasible solution for treating offshore crude oil leakage and purifying oily domestic sewage.
(5) In the process of preparing the polyformaldehyde microfiber material, the chemical structure of polyformaldehyde is not damaged, and the chemical stability of polyformaldehyde is not lost in the preparation process, so that the polyformaldehyde microfiber material can resist the separation of various oils and organic solvents. While chemical stability has a significant contribution to the recycling of the material. Therefore, as shown in fig. 5 to 8, in the oil-water separation application, the polyformaldehyde microfiber has long service life, and can still maintain ultrahigh air and oil water contact angles, oil adsorption capacity and oil-water separation effect after being repeatedly recycled for 10 times. Meanwhile, after the material is used, the material can be subjected to smashing, dispersing, washing, filtering and the like again to prepare a recycled polyformaldehyde microfiber material which is reused for oil-water separation, and the recycled polyformaldehyde microfiber material still has high air and oil water contact angles, oil adsorption capacity and oil-water separation efficiency in 10 times of recycling, so that the cost and time of oil-water separation are greatly reduced, the recycling and the reutilization are realized, and the social and economic benefits are high.
Drawings
FIG. 1 is a photomicrograph of the polyoxymethylene microfiber prepared in example 4.
Fig. 2 (a) (b) is a sectional SEM topography of the polyoxymethylene nascent fibers in the comparative example and the drawn fibers in example 4, and fig. 2 (c) (d) is a SEM topography of polyoxymethylene powder prepared from the polyoxymethylene nascent fibers and polyoxymethylene microfibers prepared from the polyoxymethylene drawn fibers.
Fig. 3 is one-dimensional and two-dimensional XRD patterns of the polyoxymethylene primary fibers in the comparative example and the polyoxymethylene drawn fibers in example 4.
FIG. 4 is the air-water contact angles of the polyoxymethylene microfiber films of examples 1 to 6, in which the mechanical shear pulverization and disassembly time was 5 minutes, 10 minutes, 30 minutes, 50 minutes, 90 minutes and 120 minutes, respectively.
Fig. 5 (a) is the contact angle of water in air, oil (chloroform and cyclohexane) of the polyoxymethylene microfiber of example 4 recycled 10 times, and fig. 5 (b) is the contact angle of water in air, oil (chloroform and cyclohexane) of the recycled polyoxymethylene microfiber of example 4 recycled 10 times.
Fig. 6 (a) is the amount of adsorption of various oils and organic solvents by the polyoxymethylene microfiber in example 4, and fig. 6 (b) is the amount of adsorption of various oils and organic solvents by the recovered polyoxymethylene microfiber in example 4.
FIG. 7 shows the oil (chloroform and cyclohexane) adsorption amounts of the polyoxymethylene microfibers in example 4 recycled 10 times.
Fig. 8 (a) shows the oil-water separation and continuity separation efficiency of the polyoxymethylene microfibers in example 4 after being recycled 10 times, and fig. 8 (b) shows the oil-water separation and continuity separation efficiency of the recovered polyoxymethylene microfibers in example 4 after being recycled 10 times.
Fig. 9 (a) is a photograph of the polyoxymethylene microfiber molded into various shapes in example 4, and fig. 9 (b) is a homemade self-supporting polyoxymethylene microfiber oil-water separation cup which can be used for continuous oil-water separation.
Comparative example
The temperatures of 6 heating zones of a screw rod of a spinning machine are respectively setPreheating at 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃ for 1 hour, then pouring polyformaldehyde granules into a storage bin for melting, starting winding when a melt flows out of a spinneret plate of a spinning assembly, wherein the winding speed of a winding machine is 300rpm, and the frequency of a reciprocating shaft is 200Hz, so as to obtain polyformaldehyde nascent fibers, and obtain the non-stretch-ratio polyformaldehyde nascent fibers. And then, cutting the polyformaldehyde nascent fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. Pulverizing time 50 min, shear rate 10 5 s -1 . After shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde powder water dispersion, washing with deionized water for 3 times, and then putting into a drying oven at 70 ℃ for drying for 10 hours to obtain polyformaldehyde powder.
The polyoxymethylene powder obtained in this example had a porosity of 56.4% and exhibited a flake structure without a microfiber morphology. The polyformaldehyde powder material of the example is subjected to suction filtration to form a film, and the test result shows that the air-water contact angle value is 70 degrees, the water contact angle in oil (chloroform and cyclohexane) cannot be measured, the adsorption capacity to (chloroform) is 8.9 times due to the fact that the polyformaldehyde powder is too loose, and the water separation efficiency of the oil (chloroform and cyclohexane) is 88.3 percent.
Example 1
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃ and preheated for 1 hour, then polyoxymethylene granules are poured into a stock bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of the spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so as to obtain the polyformaldehyde nascent fiber, and then carrying out air hot drawing on the polyformaldehyde nascent fiber, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 700rpm, that is, the draw ratio was 7 times.
And then, cutting the obtained polyformaldehyde drawn fibers to 2cm by using a cutter to obtain cut fibers, putting the cut fibers into a mechanical crusher, adding 2 liters of water, and performing mechanical shearing, crushing and disassembling. The crushing time is 5 minutesShear rate of 10 5 s -1 . And after shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then drying in an oven at 70 ℃ for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 70.2%, a diameter of about 30 to 35 μm and a length of about 110 to 130 μm. The polyformaldehyde microfiber material of the example is subjected to suction filtration to form a film, and the test result shows that the value of an air-water contact angle is 93 degrees, the water contact angle in oil (chloroform and cyclohexane) is 155 degrees, the adsorption amount on the (chloroform) is 16.6 times, and the water separation efficiency of the oil (chloroform and cyclohexane) is 89.8%.
Example 2
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, and after preheating is carried out for 1 hour, polyformaldehyde granules are poured into a storage bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of the spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so as to obtain the polyformaldehyde nascent fiber, and then carrying out air hot drawing on the polyformaldehyde nascent fiber, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 700rpm, that is, the draw ratio was 7 times.
And then, cutting the obtained polyformaldehyde stretched fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. Pulverizing time of 10 min and shear rate of 10 5 s -1 . After shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then putting into a drying oven at 70 ℃ for drying for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 76.4%, a diameter of about 20 to 25 μm, and a length of about 110 to 120 μm. The polyoxymethylene microfiber material of this example was suction filtered into a film, and the test showed that the air-water contact angle value was 109 °, the water contact angle in oil (chloroform and cyclohexane) was 156 °, the adsorption amount to (chloroform) was 17.8 times, and the oil (chloroform and cyclohexane) water separation efficiency was 95.6%.
Example 3
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, and after preheating is carried out for 1 hour, polyformaldehyde granules are poured into a storage bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of the spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so as to obtain the polyformaldehyde nascent fiber, and then carrying out air hot drawing on the polyformaldehyde nascent fiber, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 700rpm, that is, the draw ratio was 7 times.
And then, cutting the obtained polyformaldehyde stretched fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. The crushing time was 30 minutes and the shear rate was 10 5 s -1 . And after shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then drying in an oven at 70 ℃ for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 82.9%, a diameter of about 10 to 20 μm, and a length of about 100 to 110 μm. The polyformaldehyde microfiber material of the example is subjected to suction filtration to form a film, and the test result shows that the air-water contact angle value is 125 degrees, the water contact angle in oil (chloroform and cyclohexane) is 158 degrees, the adsorption amount to the (chloroform) is 18.6 times, and the water separation efficiency of the oil (chloroform and cyclohexane) is 96.4%.
Example 4
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, and after preheating is carried out for 1 hour, polyformaldehyde granules are poured into a storage bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of a spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so that the polyformaldehyde nascent fiber is obtained, and then the polyformaldehyde nascent fiber is subjected to air hot drawing, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 700rpm, that is, the draw ratio was 7 times.
And then, cutting the obtained polyformaldehyde stretched fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. The crushing time was 50 minutes and the shear rate was 10 5 s -1 . And after shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then drying in an oven at 70 ℃ for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 89.1%, a diameter of about 10 to 20 μm, and a length of about 80 to 100 μm. The polyoxymethylene microfiber material prepared in the example is filtered into a film, and the water contact angles of air and oil (chloroform and cyclohexane) are 131 degrees and 160 degrees after testing, and the water contact angles of air after 10 times of recycling are maintained at about 130 degrees and 160 degrees, which are basically the same as the initial test results (fig. 5). The adsorption amounts of the polyoxymethylene microfibers to various oils and organic solvents were as shown in fig. 6 and 7, and the adsorption amount to chloroform was the highest and 19.5 times, and the adsorption amount to oils (chloroform and cyclohexane) after 10 cycles of use did not change much. As shown in fig. 8, the polyoxymethylene microfiber material has an oil (chloroform) water separation and continuous oil-water separation efficiency of 99% or more after 10 cycles of recycling. As shown in fig. 9, the polyoxymethylene microfiber material can be plasticized by various molds, and can be self-made into a self-supporting continuous oil-water separation cup, thereby realizing efficient oil-water separation.
The used polyformaldehyde microfiber is dispersed in 1L water at 10000rpm, and filtered to obtain recycled polyformaldehyde microfiber material, and the water contact angle, oil adsorption amount and oil-water separation efficiency of air and oil which are tested and recycled for 10 times are shown in figures 5, 6 and 8 respectively.
Example 5
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, and after preheating is carried out for 1 hour, polyformaldehyde granules are poured into a storage bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of the spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so as to obtain the polyformaldehyde nascent fiber, and then carrying out air hot drawing on the polyformaldehyde nascent fiber, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 700rpm, that is, the draw ratio was 7 times.
And then, cutting the obtained polyformaldehyde stretched fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. The crushing time was 90 minutes and the shear rate was 10 5 s -1 . And after shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then drying in an oven at 70 ℃ for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 83.7%, a diameter of about 10 to 15 μm, and a length of about 70 to 80 μm. The polyoxymethylene microfiber material of this example was suction filtered to form a film, and the test showed that the value of the contact angle between air and water was 121 °, the contact angle between water in oil (chloroform and cyclohexane) was 159 °, the adsorption amount to (chloroform) was 19.3 times, and the separation efficiency of water in oil (chloroform and cyclohexane) was 99.2%.
Example 6
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, and after preheating is carried out for 1 hour, polyformaldehyde granules are poured into a storage bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of the spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so as to obtain the polyformaldehyde nascent fiber, and then carrying out air hot drawing on the polyformaldehyde nascent fiber, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 700rpm, that is, the draw ratio was 7 times.
And then, cutting the obtained polyformaldehyde drawn fibers to 2cm by using a cutter to obtain cut fibers, putting the cut fibers into a mechanical crusher, adding 2 liters of water, and performing mechanical shearing, crushing and disassembling. The crushing time was 120 minutes and the shear rate was 10 5 s -1 . And after shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then drying in an oven at 70 ℃ for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 81.8%, a diameter of about 5 to 10 μm and a length of about 50 to 60 μm. The polyoxymethylene microfiber material of the example was suction-filtered to form a film, and the test results showed that the air-water contact angle value was 121 °, the water contact angle in oil (chloroform and cyclohexane) was 158 °, the adsorption amount to (chloroform) was 19.0 times, and the water separation efficiency of oil (chloroform and cyclohexane) was 99.2%.
Example 7
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃, and after preheating is carried out for 1 hour, polyformaldehyde granules are poured into a storage bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of a spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so that the polyformaldehyde nascent fiber is obtained, and then the polyformaldehyde nascent fiber is subjected to air hot drawing, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 500rpm, that is, the draw ratio was 5 times.
And then, cutting the obtained polyformaldehyde stretched fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. The crushing time was 50 minutes and the shear rate was 10 5 s -1 . After shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then putting into a drying oven at 70 ℃ for drying for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 85.5%, a diameter of about 15 to 25 μm, and a length of about 80 to 90 μm. The polyformaldehyde microfiber material of the example is subjected to suction filtration to form a film, and the test result shows that the value of an air-water contact angle is 120 degrees, the water contact angle in oil (chloroform and cyclohexane) is 156 degrees, the adsorption amount on the (chloroform) is 19.0 times, and the water separation efficiency of the oil (chloroform and cyclohexane) is 90.4%.
Example 8
The temperature of 6 heating zones of a screw of a spinning machine is respectively set to be 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃ and preheated for 1 hour, then polyoxymethylene granules are poured into a stock bin for melting, the rotating speed of a single screw of an extruder is 90rpm, and the rotating speed of a metering pump is 60rpm. And (2) starting winding when the melt flows out of a spinneret plate of the spinning component, wherein the winding speed of a winding machine is 300rpm, the frequency of a reciprocating shaft is 200Hz, so as to obtain the polyformaldehyde nascent fiber, and then carrying out air hot drawing on the polyformaldehyde nascent fiber, wherein the temperatures of 3 zones are 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber was 100rpm, and the winding speed of the polyoxymethylene drawn fiber after hot drawing was 900rpm, that is, the draw ratio was 9 times.
And then, cutting the obtained polyformaldehyde stretched fibers to 2cm by using a cutter to obtain chopped fibers, putting the chopped fibers into a mechanical crusher, adding 2 liters of water, and carrying out mechanical shearing, crushing and disassembling. The crushing time was 50 minutes and the shear rate was 10 5 s -1 . And after shearing, crushing and disassembling, carrying out suction filtration on the obtained polyformaldehyde microfiber water dispersion, washing with deionized water for 3 times, and then drying in an oven at 70 ℃ for 10 hours to obtain the polyformaldehyde microfiber oil-water separation material.
This example gives polyoxymethylene microfibers having a porosity of 84.6%, a diameter of about 10 to 20 μm, and a length of about 85 to 100 μm. The polyformaldehyde microfiber material of the example is subjected to suction filtration to form a film, and the test result shows that the value of an air-water contact angle is 123 degrees, the water contact angle in oil (chloroform and cyclohexane) is 157 degrees, the adsorption amount on the (chloroform) is 18.6 times, and the water separation efficiency of the oil (chloroform and cyclohexane) is 96.1 percent.
TABLE 1 comparative examples and various parameters and experimental results of the examples
Claims (6)
1. A polyformaldehyde microfiber oil-water separation material and a preparation method thereof are characterized by comprising the following steps:
(1) Adding the polyformaldehyde granules into a screw extruder of spinning equipment for spinning, obtaining polyformaldehyde nascent fibers without stretching multiplying power through melt spinning, then drafting the polyformaldehyde nascent fibers in an air drafting machine, and obtaining polyformaldehyde stretched fibers after winding through a winding machine;
(2) Cutting the polyformaldehyde stretched fibers obtained in the step (1) by using a cutter to obtain polyformaldehyde short fibers, putting the polyformaldehyde short fibers into a mechanical crusher, adding water, performing mechanical shearing and crushing, and disassembling to obtain a polyformaldehyde microfiber water dispersion;
(3) And (3) carrying out suction filtration on the polyformaldehyde microfiber water dispersion obtained in the step (2), washing with deionized water, and then putting into an oven for drying to finally obtain the polyformaldehyde microfiber oil-water separation material for experiments and tests.
2. The polyoxymethylene microfiber oil-water separation material and the preparation method thereof as claimed in claim 1, wherein the microfiber has a diameter ranging from 5 to 35 μm and a length ranging from 50 to 130 μm, the polyoxymethylene microfiber oil-water separation material prepared by suction filtration has an air water contact angle ranging from 90 ° to 130 °, a porosity of about 70% to 90%, a water contact angle in oil (chloroform and cyclohexane) ranging from 155 ° to 160 °, an oil (chloroform) adsorption amount ranging from 16 to 20 times, and an oil (chloroform) water separation efficiency ranging from 90% to 99.5%.
3. The polyoxymethylene microfiber oil-water separation material and the preparation method thereof according to claim 1, wherein the screw of the spinning machine in step (1) is a single screw extruder, the rotation speed of the extruder screw is 90rpm, and the temperatures of the 1-6 zones are 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃ and 210 ℃. The rotating speed of the metering pump is 60rpm, the winding speed of the winding machine is 300rpm, and the frequency of the reciprocating shaft is 200Hz.
4. The polyoxymethylene microfiber oil-water separation material and the preparation method thereof according to claim 1, wherein the temperature of 3 zones of the hot drawing process of step (1) is 100 ℃,110 ℃ and 120 ℃. The unwinding speed of the polyoxymethylene nascent fiber is 100rpm, the winding speed of the drawn fiber is 500-1000 rpm, and the drawing ratio is 5-10 times.
5. The polyoxymethylene microfiber oil-water separation material and the preparation method thereof according to claim 1, wherein the chopped fiber prepared in the step (2) has a length of 2cm. The proportion relation of the mass of the polyformaldehyde fibers added in the processes of mechanical shearing, crushing and disassembling and the added deionized water is that 10g of the fibers correspond to 2 liters of the deionized water, and the shearing rate is 10 5 s -1 The time is 5 to 120 minutes.
6. The polyoxymethylene microfiber oil-water separation material and process of claim 1, wherein in step (3), the deionized water is washed 3 times, the oven drying temperature is 70 ℃, and the drying time is 10 hours.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002146637A (en) * | 2000-11-02 | 2002-05-22 | Unitika Ltd | Method for producing polyoxymethylene fiber |
| WO2009085679A1 (en) * | 2007-12-28 | 2009-07-09 | 3M Innovative Properties Company | Composite nonwoven fibrous webs and methods of making and using the same |
| CN101792938A (en) * | 2010-04-01 | 2010-08-04 | 东华大学 | Novel preparation technology of polyoxymethylene fiber |
| WO2011133396A1 (en) * | 2010-04-22 | 2011-10-27 | 3M Innovative Properties Company | Nonwoven fibrous webs containing chemically active particulates and methods of making and using same |
| CN102872833A (en) * | 2011-07-13 | 2013-01-16 | 冯淑芹 | Novel ion exchange fiber and its application |
| CN105177756A (en) * | 2015-10-27 | 2015-12-23 | 开滦（集团）有限责任公司 | Method for preparing polyformaldehyde nascent fibers |
| CN105603637A (en) * | 2016-01-19 | 2016-05-25 | 南京林业大学 | Efficient electrostatic spinning oil-water separation fiber membrane |
| CN105906909A (en) * | 2016-05-18 | 2016-08-31 | 郑州大学 | High-density polyethylene oil-water separation material and preparation method thereof |
| CN107875673A (en) * | 2016-09-29 | 2018-04-06 | 南京林业大学 | A kind of preparation method of superhydrophilic superoleophobic type nano fibrous membrane |
| US20210101120A1 (en) * | 2019-10-04 | 2021-04-08 | Research & Business Foundation Sungkyunkwan University | Semipermeable membrane for waiter treatment, preparing method for the same, and polluted water treatment system including the same |
-
2022
- 2022-09-27 CN CN202211182380.6A patent/CN115722209B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002146637A (en) * | 2000-11-02 | 2002-05-22 | Unitika Ltd | Method for producing polyoxymethylene fiber |
| WO2009085679A1 (en) * | 2007-12-28 | 2009-07-09 | 3M Innovative Properties Company | Composite nonwoven fibrous webs and methods of making and using the same |
| CN101792938A (en) * | 2010-04-01 | 2010-08-04 | 东华大学 | Novel preparation technology of polyoxymethylene fiber |
| WO2011133396A1 (en) * | 2010-04-22 | 2011-10-27 | 3M Innovative Properties Company | Nonwoven fibrous webs containing chemically active particulates and methods of making and using same |
| CN102872833A (en) * | 2011-07-13 | 2013-01-16 | 冯淑芹 | Novel ion exchange fiber and its application |
| CN105177756A (en) * | 2015-10-27 | 2015-12-23 | 开滦（集团）有限责任公司 | Method for preparing polyformaldehyde nascent fibers |
| CN105603637A (en) * | 2016-01-19 | 2016-05-25 | 南京林业大学 | Efficient electrostatic spinning oil-water separation fiber membrane |
| CN105906909A (en) * | 2016-05-18 | 2016-08-31 | 郑州大学 | High-density polyethylene oil-water separation material and preparation method thereof |
| CN107875673A (en) * | 2016-09-29 | 2018-04-06 | 南京林业大学 | A kind of preparation method of superhydrophilic superoleophobic type nano fibrous membrane |
| US20210101120A1 (en) * | 2019-10-04 | 2021-04-08 | Research & Business Foundation Sungkyunkwan University | Semipermeable membrane for waiter treatment, preparing method for the same, and polluted water treatment system including the same |
Non-Patent Citations (3)
| Title |
|---|
| MENGXIN ZHAO等: "Facile preparation of superhydrophobic porous wood for continuous oilwater separation", 《JOURNAL OF WATER PROCESS ENGINEERING》, vol. 36, pages 101279 * |
| WENBIN JIN等: "Preparation of recyclable and deformable POM microfiber for oil–water separation with nature-inspired top–bottom strategy", 《CHEMICAL ENGINEERING JOURNAL 》, vol. 458, pages 143332 * |
| 李建华等: "二步法制备高强度聚甲醛纤维的工艺及性能研究", 《合成纤维工业》, vol. 42, no. 6, pages 7 - 10 * |
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