CN115852743A - High-compressibility and flame-retardant carbon fiber oil absorbent felt and preparation method thereof - Google Patents
High-compressibility and flame-retardant carbon fiber oil absorbent felt and preparation method thereof Download PDFInfo
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- CN115852743A CN115852743A CN202211528808.8A CN202211528808A CN115852743A CN 115852743 A CN115852743 A CN 115852743A CN 202211528808 A CN202211528808 A CN 202211528808A CN 115852743 A CN115852743 A CN 115852743A
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- carbon fiber
- felt
- polyphenylene sulfide
- oil absorbent
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 44
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 44
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 230000002745 absorbent Effects 0.000 title claims abstract description 36
- 239000002250 absorbent Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000003063 flame retardant Substances 0.000 title claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 60
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 54
- 239000000835 fiber Substances 0.000 claims description 23
- 239000004745 nonwoven fabric Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 238000010521 absorption reaction Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010494 dissociation reaction Methods 0.000 claims description 3
- 230000005593 dissociations Effects 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 238000004537 pulping Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 abstract description 34
- 239000010779 crude oil Substances 0.000 abstract description 17
- 238000003466 welding Methods 0.000 abstract description 7
- 238000004140 cleaning Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 description 4
- 230000003075 superhydrophobic effect Effects 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 238000010009 beating Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 244000000626 Daucus carota Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000238634 Libellulidae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 235000005770 birds nest Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
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- 239000002002 slurry Substances 0.000 description 1
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- 239000013589 supplement Substances 0.000 description 1
- 235000005765 wild carrot Nutrition 0.000 description 1
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Abstract
The invention relates to a high compressibility and flame retardant carbon fiber oil absorbent felt and a preparation method thereof. The welding point of the oil absorbent felt obtained by the preparation method of the invention hinders the interface slippage under the external load, so that the absorbent has strong cyclic compressibility. The absorbent exhibits exceptional hydrophobicity and excellent fire resistance without further hydrophobic modification or the addition of any flame retardant. Meanwhile, the continuous conductive network enables the absorbent to have very high photo-thermal and joule heating effects, thereby improving the adsorption efficiency of the crude oil through the self-heating function. The preparation method is simple and environment-friendly, does not use any organic solvent, and is expected to provide a good solution for all-weather cleaning of crude oil leakage in severe environment.
Description
Technical Field
The invention relates to the field of preparation methods of functional polymer materials, in particular to a high-compressibility and flame-retardant carbon fiber oil-absorbing felt and a preparation method thereof.
Background
The frequent occurrence of accidents of crude oil leakage during offshore oil exploration and transportation causes catastrophic damages to the ocean safety and ecological balance as well as human health. Currently, various techniques reported in the literature (such as dispersants, in situ combustion, biodegradation, absorption, and skimmers) have been used to treat crude oil leaks. Among them, the adsorption route of hydrophobic and lipophilic adsorbents is simple, green and free from secondary pollution, and is considered as the most promising adsorption strategy. However, the extremely high viscosity of the crude oil prevents them from diffusing into the interior of the absorbent, resulting in poor cleaning and recovery of the crude oil. Therefore, it remains very challenging to develop an advanced crude oil spill remediation absorbent. It is known that increasing the temperature of crude oil is an effective way to reduce the viscosity of crude oil, and from this point of view, it is necessary to design an absorbent with photothermal and/or joule heating functions. Under the condition of the photo-thermal conversion adsorbent, solar energy can be captured and then converted into heat to heat surrounding crude oil, and when the solar energy is weak or difficult to obtain, the Joule heating absorbent can be used as a supplement to convert electric energy into Joule heat to realize all-weather cleaning of crude oil leakage. In addition, crude oil is highly flammable. In the desorption and recovery process, the high temperature generated by photo-thermal heating or Joule heating easily causes the combustion of crude oil, and brings more serious pollution problem. Inspired by bird's nest, we propose a novel polymer welding strategy, utilize polyphenylene sulfide (PPS) welding carbon fiber to prepare a high compressibility and fire-resistant oil absorption felt, polyphenylene sulfide (PPS) is an ideal welding material, can make discontinuous carbon fiber material interconnect, form porous integral structure. The obtained oil absorption felt shows stable super-hydrophobic and lipophilic behaviors even under strong acid and strong alkali conditions without further treatment, and the mutually connected welding structure ensures that the oil absorption felt has strong compressibility and higher photo-thermal and Joule heating effects.
Disclosure of Invention
The invention aims to solve the technical problems and requirements and provides a high-compressibility and flame-retardant carbon fiber oil absorbent felt and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a high-compressibility and flame-retardant carbon fiber oil absorbent felt comprises the following steps:
and 3, mixing the carbon fiber cleaned in the step 1 with the polyphenylene sulfide non-woven fabric fiber pulp obtained in the step 2 according to the ratio of (4-6): (4-6), and treating the mixture by using a pulp disintegrator to obtain a mixture after dissociation treatment;
and 5, filtering for multiple times by adopting a wet papermaking method to obtain the original felt.
And 6, drying and heating the original felt, and carbonizing to obtain the well-carbonized oil absorption felt.
Further, the step 1 specifically comprises: the polyphenylene sulfide non-woven fabric and the carbon fiber are respectively added into an acetone solution, residual stains and dust are removed by ultrasonic waves, and the mixture is dried in a vacuum furnace at the temperature of 80 ℃.
Further, in the step 3, the mass ratio of the polyphenylene sulfide nonwoven fabric to the carbon fiber is 4.
Further, the aqueous dispersion in the step 4 comprises polyethylene oxide and anionic polyacrylamide in a mass ratio of 6.
Further, the step 6 specifically includes the following steps: drying the original felt at 120 ℃, then forming at 300 ℃, finally heating to 800 ℃ in a tube furnace at the speed of 10 ℃/s, keeping at the temperature for 2 hours, and then continuously cooling to room temperature at the speed of 10 ℃/s to obtain the carbonized oil absorption felt.
Further, the length of the carbon fiber is chopped fiber with any size.
Further, in the step 4, stirring is performed until the polyethylene oxide is not agglomerated, and the stirring time is 3 to 8 hours.
The carbon fiber oil absorbent felt with high compressibility and flame retardance is prepared by the method.
After the technical scheme is adopted, compared with the prior art, the invention has the following advantages:
the invention adopts a wet papermaking method, provides a polymer 'welding' strategy, designs a multifunctional absorbent, and connects discontinuous carbon fibers together to form a three-dimensional welding structure by adopting polyphenylene sulfide (PPS) as an adhesive, and tests show that the oil absorption felt has good resilience and excellent oil absorption capacity only when the mass ratio of the mixture of the polyphenylene sulfide (PPS) and the carbon fibers is 5.
Due to the Presence of Polyphenylene Sulfide (PPS) and carbon fibers, the oil absorbent felt has ultra-light, super-hydrophobic, compressible and flame retardant properties without any treatment, and better photo-thermal and Joule heating effects. These excellent properties will allow the oil felt of the present invention to be used on a large scale for safely and effectively cleaning and recovering crude oil spills in harsh environments.
Compared with the traditional method, the method has the following advantages: 1) The preparation process is simple and can be prepared on a large scale; 2) The product has the advantages of super-light, super-hydrophobic, compressible and flame retardant properties, and better photo-thermal and Joule heating effects without any treatment; 3) The composite material can be used in severe environment, and both polyphenylene sulfide (PPS) and carbon fiber have good corrosion resistance. Therefore, the oil absorbent felt prepared by the method can be applied to the efficient cleaning and recovery of crude oil leakage in severe environment in a large scale.
The present invention will be described in detail below with reference to the drawings and examples.
Drawings
FIG. 1 is a flow chart of the preparation of the oil absorbent felt of the present invention;
FIG. 2 is a diagram of super-hydrophobic and oleophilic contact angle and substance of the oil absorbent felt of the present invention;
FIG. 3 is a graph of the temperature of the oil absorbent felt of the present invention under different illumination intensities along with time;
FIG. 4 is the maximum oil absorption capacity and speed of the oil absorbent felt of the present invention at different voltages for crude oil;
fig. 5 is a schematic view of the flame retardancy of the oil absorbent felt of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
Respectively adding Carbon Fiber (CFS) and polyphenylene sulfide (PPS) superfine fiber nonwoven fabrics into an acetone solution, removing residual stains and dust by ultrasonic waves, and drying in a vacuum furnace at 80 ℃. Polyphenylene Sulfide (PPS) nonwoven fabric was beaten with a beater for 60min to produce polyphenylene sulfide fiber pulp. Polyphenylene sulfide fiber pulp was mixed with Carbon Fiber (CFS) at a mass ratio of 4. Preparing an aqueous dispersion, adding PEO: APAM = 6. After being uniformly mixed, the mixture is filtered for many times by adopting a wet papermaking method to obtain a wet original felt. Drying at 120 ℃, forming at 300 ℃, heating to 800 ℃ in a tube furnace at the speed of 10 ℃/s, keeping at the temperature for 2 hours, and continuously cooling to room temperature at the speed of 10 ℃/s to obtain the carbonized oil absorbent felt.
Example 2
Respectively adding Carbon Fiber (CFS) and polyphenylene sulfide (PPS) superfine fiber nonwoven fabrics into an acetone solution, removing residual stains and dust by ultrasonic waves, and drying in a vacuum furnace at 80 ℃. Polyphenylene Sulfide (PPS) nonwoven fabric was beaten with a beater for 60min to produce polyphenylene sulfide fiber pulp. Polyphenylene sulfide fiber pulp was mixed with Carbon Fiber (CFS) at a mass ratio of 5. Preparing an aqueous dispersion, wherein the mass ratio of PEO: APAM =6, solute of 1 as a dispersant, stirred for several hours, and then the resulting mixture was transferred to a dispersion. After being uniformly mixed, the mixture is filtered for many times by adopting a wet papermaking method to obtain a wet original felt. Drying at 120 ℃, forming at 300 ℃, heating to 800 ℃ in a tube furnace at the speed of 10 ℃/s, keeping at the temperature for 2 hours, and continuously cooling to room temperature at the speed of 10 ℃/s to obtain the carbonized oil absorbent felt.
Example 3
Respectively adding Carbon Fiber (CFS) and polyphenylene sulfide (PPS) superfine fiber nonwoven fabrics into an acetone solution, removing residual stains and dust by ultrasonic waves, and drying in a vacuum furnace at 80 ℃. Polyphenylene Sulfide (PPS) nonwoven fabric was beaten with a beater for 60min to produce polyphenylene sulfide fiber pulp. Polyphenylene sulfide fiber pulp was mixed with Carbon Fiber (CFS) in a mass ratio of 6. Preparing an aqueous dispersion, adding PEO: APAM =6, solute of 1 as a dispersant, stirred for several hours, and then the resulting mixture was transferred to a dispersion. After being uniformly mixed, the mixture is filtered for many times by adopting a wet papermaking method to obtain a wet original felt. Drying at 120 ℃, forming at 300 ℃, heating to 800 ℃ in a tube furnace at the speed of 10 ℃/s, keeping at the temperature for 2 hours, and continuously cooling to room temperature at the speed of 10 ℃/s to obtain the carbonized oil absorbent felt.
By three examples, it is shown that the polyphenylene sulfide fiber slurry is mixed with Carbon Fiber (CFS) at a mass ratio of 5. On the one hand, as the polyphenylene sulfide fiber pulp increases, excess polyphenylene sulfide (PPS) melts on the carbon fibers rather than at the junctions, which causes voids between the carbon fibers to be occupied, resulting in low oil adsorption capacity; on the other hand, if the amount of polyphenylene sulfide fiber pulp is insufficient, part of the carbon fibers cannot be connected together, which results in unstable structure. Therefore, the mixing of the polyphenylene sulfide fiber pulp with the Carbon Fiber (CFS) in a mass ratio of 5.
FIG. 1 shows a flow chart of the preparation of PPS @ CFS of the present invention. Cleaning and drying Carbon Fiber (CFS) and polyphenylene sulfide (PPS) superfine fiber non-woven fabric, and beating the polyphenylene sulfide (PPS) non-woven fabric into polyphenylene sulfide fiber pulp by using a beating machine. Polyphenylene sulfide fiber pulp and Carbon Fiber (CFS) are mixed according to a certain mass ratio and then are dissociated into separated fibers in a pulp dissociation machine. Preparing an aqueous dispersion, adding a certain mass ratio of PEO and APAM as a dispersing agent, stirring for several hours, and then transferring the obtained mixture into the dispersion. After being uniformly mixed, the mixture is filtered for many times by adopting a wet papermaking method to obtain a wet original felt. Drying at 120 deg.C, shaping at 300 deg.C, heating to 800 deg.C in a tube furnace, holding at the temperature for 2 hr, and cooling to room temperature to obtain carbonized oil absorbent felt.
As shown in FIG. 2, the Water Contact Angle (WCA) of PPS @ CFS reached 152 °, the oil contact angle was 0 °, and a significant mirror surface phenomenon was observed after immersing PPS @ CFS in water.
As shown in FIG. 3, the intensity of irradiation with the sun was from 1.0kW/m 2 Increased to 3.0kW/m 2 The surface equilibrium temperature of PPS @ CFS oil absorbent felt is gradually increased from 68 ℃ to 1After the lamp is turned off at 20 ℃, the PPS @ CFS oil absorbent felt is rapidly cooled to the room temperature.
As shown in figure 4, the maximum oil absorption capacity and the oil velocity of the crude oil reach 45gg respectively under the voltage of 5V -1 And 5.2mL cm -3 s -1 。
As shown in FIG. 5, the PPS @ CFS oil absorbent felt was unable to burn in normal atmosphere when placed directly on the alcohol burner flame, indicating its non-flammability.
The foregoing is illustrative of the best mode of the invention and details not described herein are within the common general knowledge of a person of ordinary skill in the art. The scope of the present invention is defined by the appended claims, and any equivalent modifications based on the technical teaching of the present invention are also within the scope of the present invention.
Claims (8)
1. The preparation method of the high-compressibility and flame-retardant carbon fiber oil absorbent felt is characterized by comprising the following steps of:
step 1, polyphenylene sulfide non-woven fabric and carbon fiber are cleaned and dried;
step 2, pulping the polyphenylene sulfide non-woven fabric cleaned in the last step for 50-70min to obtain polyphenylene sulfide non-woven fabric fiber pulp;
and 3, mixing the carbon fibers cleaned in the step 1 with the polyphenylene sulfide non-woven fabric fiber pulp obtained in the step 2 according to the ratio of (4-6): (4-6), and treating the mixture by using a pulp disintegrator to obtain a mixture after dissociation treatment;
step 4, preparing aqueous dispersion liquid, transferring the dissociated mixture obtained in the step 3 into the dispersion liquid, and uniformly mixing;
and 5, filtering for multiple times by adopting a wet papermaking method to obtain the original felt.
And 6, drying and heating the original felt, and carbonizing to obtain the well-carbonized oil absorption felt.
2. The method for preparing the high compressibility and flame retardancy carbon fiber oil absorbent felt according to claim 1, wherein the step 1 is specifically: respectively adding the polyphenylene sulfide non-woven fabric and the carbon fiber into an acetone solution, removing residual stains and dust by using ultrasonic waves, and drying in a vacuum furnace at the temperature of 80 ℃.
3. The method for preparing the high compressibility and flame retardancy carbon fiber oil absorbent felt according to claim 1, wherein in the step 3, the mass ratio of the polyphenylene sulfide nonwoven fabric to the carbon fiber is 4.
4. The method for preparing the high compressibility and flame retardancy carbon fiber oil absorbent felt according to claim 3, wherein the aqueous dispersion in the step 4 comprises polyethylene oxide and anionic polyacrylamide in a mass ratio of 6.
5. The method for preparing the high compressibility and flame retardancy carbon fiber oil absorbent felt according to claim 3, wherein the step 6 specifically comprises the following steps: drying the original felt at 120 ℃, then forming at 300 ℃, finally heating to 800 ℃ in a tube furnace at the speed of 10 ℃/s, keeping at the temperature for 2 hours, and then continuously cooling to room temperature at the speed of 10 ℃/s to obtain the carbonized oil absorption felt.
6. The method for preparing a high compressibility and flame retardancy carbon fiber oil absorbent felt according to claim 3, wherein the length of the carbon fiber is chopped fiber of any size.
7. The method for preparing a high compressibility and flame retardancy carbon fiber oil absorbent felt according to claim 3, wherein in the step 4, the stirring is performed until the polyethylene oxide is not agglomerated, and the stirring time is 3 to 8 hours.
8. Highly compressible and flame retardant carbon fiber oil felt, characterized in that it is prepared by the process according to any one of claims 1 to 7.
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