CN111228858B - Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber - Google Patents
Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber Download PDFInfo
- Publication number
- CN111228858B CN111228858B CN202010097501.1A CN202010097501A CN111228858B CN 111228858 B CN111228858 B CN 111228858B CN 202010097501 A CN202010097501 A CN 202010097501A CN 111228858 B CN111228858 B CN 111228858B
- Authority
- CN
- China
- Prior art keywords
- carbon fiber
- nickel
- super
- cleaning
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 91
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 91
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000009713 electroplating Methods 0.000 claims abstract description 29
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002791 soaking Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 8
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003292 glue Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- 238000012545 processing Methods 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000007747 plating Methods 0.000 claims description 11
- 239000012935 ammoniumperoxodisulfate Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 229920002120 photoresistant polymer Polymers 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 20
- 235000019198 oils Nutrition 0.000 abstract description 16
- 235000019476 oil-water mixture Nutrition 0.000 abstract description 7
- 230000003472 neutralizing effect Effects 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract 1
- 229910001453 nickel ion Inorganic materials 0.000 abstract 1
- 238000007788 roughening Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000000295 fuel oil Substances 0.000 description 4
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000010687 lubricating oil Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- AZWHFTKIBIQKCA-UHFFFAOYSA-N [Sn+2]=O.[O-2].[In+3] Chemical compound [Sn+2]=O.[O-2].[In+3] AZWHFTKIBIQKCA-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention belongs to the technical field of functional materials, and relates to a preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber. The method plates a layer of metallic nickel on the surface of the carbon fiber through the processes of pretreatment, nickel electroplating and fluorination, and enables the carbon fiber to have super-hydrophobic performance. Pretreatment: removing glue by an acetone method, removing oil by acid-alkali liquor at high temperature, roughening the surface of the carbon fiber to enable the surface to present a rough microstructure, and finally neutralizing; electroplating nickel: immersing the dispersed carbon fibers into a solution containing nickel ions, fixing the carbon fibers on a direct-current power supply cathode, and placing the carbon fibers and the anode nickel plate in parallel and symmetrical mode; fluorination: and soaking the nickel-plated carbon fiber in a fluorosilane ethanol solution. The contact angle of the super-hydrophobic super-oleophylic nickel-plated carbon fiber to water is more than 150 degrees, and the contact angle to oil is less than 10 degrees. The method has the advantages of simplicity, easy operation, low cost and the like, and can effectively realize the high-purity separation of various oil-water mixtures.
Description
Technical Field
The invention belongs to the technical field of functional materials, and relates to a preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber.
Background
The high-purity separation technology of oil-water mixture is one of the hot problems in the engineering technical field. The large amount of the oil-water mixture is leakage of marine oil, crude oil pollution and the small amount of the oil-water mixture caused by the oil used in the home factory, which can not only destroy water quality, pollute soil and influence environment, but also easily cause huge economic loss and even harm human health. Therefore, the method has great practical significance on how to realize the oil-water separation with high purity.
The current methods for separating oil-water mixtures can be divided into conventional treatment methods and methods based on extremely wetting materials. The traditional treatment methods comprise a microbial degradation method, a combustion method, an oil collection method, a fence method, a gravity method and the like, and although the separation of an oil-water mixture can be carried out, the traditional treatment methods still have some obvious defects, such as low separation purity, secondary pollution, slow treatment speed and the like. Compared with the traditional method, the method based on the extreme wettability material is more efficient and lower in cost, but still has some problems in the preparation method of the extreme wettability material. Patent CN103626171A discloses a preparation method of graphene sponge for oil-water separation, which is characterized in that graphene solution is soaked and matched with reduction reaction, and the preparation method is complex in preparation process, very high in cost, difficult to popularize and low in practical application value. An ACS Applied Materials & Interfaces,2009,11,2613 reports a preparation method of a super-hydrophobic super-oleophylic copper mesh for oil-water separation, specifically, the super-hydrophobic super-oleophylic copper mesh is obtained by immersing a nitric acid solution on a copper mesh to construct a microstructure and then modifying the microstructure with low surface energy. Patent CN105002721B discloses a preparation method of wear-resistant super-hydrophobic cotton cloth for oil-water separation, which is obtained by reacting ethyl silicate, a silane coupling agent and ethanol under an ultrasonic condition. A paper (Chemical Communication,2005,640-642) reports a preparation method of a super-hydrophilic surface, specifically, an indium oxide-tin oxide super-hydrophilic surface is prepared on a glass substrate by an electrochemical method, the method can obtain the super-hydrophilic surface without illumination, but the prepared surface can not maintain extreme wettability for a long time and can not be stored for a long time. The article (Surface Science Reports,2008,63: 515-. The super-hydrophilic film prepared by the method can gradually change into hydrophobicity in a light environment for a long time, and cannot be used for a long time.
Therefore, there is a need to develop a method for preparing a novel material with extreme wettability for oil-water separation, which is safe, environment-friendly, simple and easy to operate, and has high durability.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber, which is safe, environment-friendly, simple and easy to operate and strong in durability, and the obtained nickel-plated carbon fiber has the advantages of wide applicability and high bonding strength of nickel plating and a matrix, and can be used for realizing oil-water separation in high purity and complex environments.
The technical scheme of the invention is as follows:
a preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber comprises the following steps:
(1) pretreatment of
Removing the photoresist by adopting an acetone method, and sequentially soaking the carbon fiber in acetone and deionized water for ultrasonic cleaning for 2-3 times; removing oil stains on the surface by using acid-alkali liquor, and ultrasonically cleaning the carbon fiber after the glue is removed by using 0.5-2 mol/L NaOH solution and 0.5-2 mol/L HCl solution in sequence, and cleaning by using deionized water; then soaking the carbon fiber with the greasy dirt removed on the surface in a mixed aqueous solution of ammonium peroxodisulfate and sulfuric acid, wherein the concentration of the ammonium peroxodisulfate is 50-300 g/L, and the concentration of the sulfuric acid is 50-200 ml/L, simultaneously carrying out ultrasonic cleaning, and then cleaning with deionized water to coarsen the surface of the carbon fiber so that the surface of the carbon fiber presents a rough microstructure; finally, NaOH solution with the mass fraction of 5% -20% is utilized for neutralization, and then deionized water is used for cleaning, so that the pretreatment process is completed; the time for removing the photoresist by the acetone cannot be less than 30min, and the time for soaking the photoresist in the mixed solution of ammonium peroxydisulfate and sulfuric acid cannot be less than 10 min.
(2) Electroplating of nickel
The components and concentrations of the plating solution are as follows: 50 g/L-300 g/L of nickel sulfate, 10 g/L-100 g/L of nickel chloride, 5 g/L-50 g/L of boric acid and 0.01 g/L-0.5 g/L of sodium dodecyl sulfate. Cutting single-beam pretreated carbon fiber to be used as a cathode, symmetrically placing the carbon fiber in parallel with an anode nickel plate with the area size not smaller than that of the cathode, connecting the anode nickel plate with a power supply through a lead, and connecting the nickel plate with the anode of the power supply and the carbon fiberConnecting a power supply cathode, then placing the power supply cathode into electroplating solution to start electroplating processing, and cleaning and drying after the electroplating processing is finished to obtain nickel-plated carbon fibers; the product of the carbon fiber electroplating processing time and the current density is not less than 50 min-mA/cm2The distance between the cathode and anode electrode plates cannot exceed 5cm, and the nickel-plated carbon fiber has a super-hydrophobic effect only when being processed in the plating solution range.
(3) Fluorination of
Soaking the nickel-plated carbon fiber processed in the step (2) in a fluorosilane ethanol solution with the mass fraction of 0.5-2%, treating for 20-60min, and drying to obtain the super-hydrophobic super-oleophylic nickel-plated carbon fiber; the drying temperature cannot be higher than 90 ℃.
Due to the adoption of the technical scheme, the invention has the following advantages:
(1) the preparation method has the advantages of simplicity, easy operation, low equipment requirement, low cost and the like;
(2) the nickel-plated carbon fiber processed by the method shows super-hydrophobicity and super-lipophilicity, and can keep the super-hydrophobicity and super-lipophilicity for 2 years for a long time; the contact angle of the super-hydrophobic super-oleophylic nickel-plated carbon fiber to water is more than 150 degrees, and the contact angle to oil is less than 10 degrees;
(3) the nickel-plated carbon fiber processed by the method not only has a super-hydrophobic effect on acid, alkali, salt, hot water and other liquid drops, but also can be used for separating a mixture of oil and water solutions, and shows high-efficiency separation capacity in a complex environment;
(4) the nickel-plated carbon fiber processed by the method has good separation effect on heavy oil such as dichloromethane and chloroform and light oil such as normal hexane, hexadecane, diesel oil, peanut oil and lubricating oil;
(5) the nickel-plated carbon fiber processed by the method has no bubbling and shedding on the surface plating layer after being tested by multiple cold and hot cycles, and shows good bonding strength of the plating layer.
Drawings
FIG. 1 is a scanning electron micrograph of a 7 μm pretreated carbon fiber obtained in example 1;
FIG. 2 is a scanning electron micrograph of 7 μm carbon fiber after nickel electroplating obtained in example 1;
FIG. 3 is a contact angle diagram of a 5 μ L water drop on the obtained super-hydrophobic nickel-plated carbon fiber;
FIG. 4 is a scanning electron micrograph of 7 μm nickel-plated carbon fiber obtained in example 2;
FIG. 5 is a scanning electron micrograph of 7 μm nickel-plated carbon fiber obtained in example 3.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1:
(1) pretreatment of
Removing the photoresist by adopting an acetone method, sequentially soaking the carbon fiber in 500mL of acetone and deionized water, and ultrasonically cleaning for 60min for 2 times; removing oil stains on the surface by using acid-alkali liquor, and ultrasonically cleaning the carbon fiber after the glue is removed by using 1mol/L NaOH solution and 1mol/L HCl solution for 20min in sequence, and cleaning the carbon fiber by using deionized water; then soaking the carbon fiber with the greasy dirt removed on the surface in a mixed aqueous solution of ammonium peroxodisulfate and sulfuric acid, wherein the concentration of the ammonium peroxodisulfate is 200g/L, the concentration of the sulfuric acid is 100ml/L, simultaneously carrying out ultrasonic cleaning for 20min, and then carrying out cleaning with deionized water; and finally, neutralizing for 20min by using NaOH with the mass fraction of 10%, and then washing by using deionized water. The carbon fiber after pretreatment is shown in fig. 1.
(2) Electroplating of nickel
The components and concentrations of the plating solution are as follows: 200g/L of nickel sulfate, 50g/L of nickel chloride, 30g/L of boric acid and 0.2g/L of sodium dodecyl sulfate are mixed to prepare an aqueous solution. Cutting a single bundle of pretreated carbon fiber into 6cm multiplied by 3cm as a cathode, symmetrically placing the carbon fiber in parallel with an anode nickel plate with the area size not smaller than the cathode, connecting the cathode nickel plate with a power supply through a lead, connecting the nickel plate with a positive electrode of the power supply and connecting the carbon fiber with a negative electrode of the power supply, then placing the carbon fiber into electroplating solution to start electroplating processing, wherein the product of the electroplating processing time of the carbon fiber and the current density is 168min mA/cm2The distance between the cathode and anode electrode plates is 2 cm; and after the electroplating processing is finished, washing with deionized water, and drying by blowing to obtain the nickel-plated carbon fiber. The carbon fiber after nickel electroplating is shown in fig. 2.
(3) Fluorination of
And (3) soaking the nickel-plated carbon fiber processed in the step (2) in a fluorosilane ethanol solution with the mass fraction of 1%, treating for 40min, and drying at the temperature of 60 ℃ to obtain the super-hydrophobic super-oleophylic nickel-plated carbon fiber.
The two bundles of carbon fibers after the electronickelling fluorination are dispersed and are tiled in a crossed mode to prepare a super-hydrophobic super-oleophylic nickel-plated carbon fiber net which is clamped between two flat-bottom hollow glass tubes to manufacture a simple oil-water mixture separating device. When the device is used for separating a heavy oil/water mixture, a vertical separation method is adopted, the mixture of 20mL of heavy oil/5 mL of water is poured into a separation device, so that the oil-water separation process can be realized, and after the separation is finished, the upper half part of the device is water and the lower half part of the device is oil; when the light oil/water mixture is separated, an inclined separation method is adopted, a mixture of 20mL of light oil/1 mL of water is poured into the device, and after the separation is finished, the upper half part of the device is water and the lower half part of the device is oil. The contact angle of a water drop on the superhydrophobic nickel-plated carbon fiber is shown in fig. 3.
The super-hydrophobic super-oleophylic nickel-plated carbon fiber prepared by the method shows a good application effect on oil-water separation. Can be normally used under various extreme conditions of high-concentration acid, alkali, salt and the like; the method can separate light and heavy oil such as normal hexane, hexadecane, diesel oil, lubricating oil, dichloromethane and the like with high purity, and the separation efficiency is over 97 percent.
Example 2:
(1) pretreatment of
Removing the photoresist by adopting an acetone method, sequentially soaking the carbon fiber in 500mL of acetone and deionized water, and ultrasonically cleaning for 30min for 2 times; removing oil stains on the surface by adopting acid-alkali liquor, ultrasonically cleaning the carbon fiber after the glue is removed by using 0.5mol/L NaOH solution and 0.5mol/L HCl solution for 20min in sequence, and cleaning by using deionized water; then soaking the carbon fiber with the greasy dirt removed on the surface in a mixed aqueous solution of ammonium peroxodisulfate and sulfuric acid, wherein the concentration of the ammonium peroxodisulfate is 50g/L, the concentration of the sulfuric acid is 50ml/L, simultaneously carrying out ultrasonic cleaning for 20min, and then cleaning with deionized water; and finally, neutralizing for 10min by using NaOH with the mass fraction of 5%, and then washing by using deionized water.
(2) Electroplating of nickel
The components of the plating solutionAnd the concentrations were as follows: 50g/L of nickel sulfate, 10g/L of nickel chloride, 5g/L of boric acid and 0.01g/L of sodium dodecyl sulfate are mixed to prepare an aqueous solution. Cutting a single bundle of pretreated carbon fiber into 6cm multiplied by 3cm as a cathode, symmetrically placing the carbon fiber in parallel with an anode nickel plate with the area size not smaller than the cathode, connecting the cathode nickel plate with a power supply through a lead, connecting the nickel plate with a positive electrode of the power supply and connecting the carbon fiber with a negative electrode of the power supply, then placing the carbon fiber into electroplating solution to start electroplating processing, wherein the product of the electroplating processing time of the carbon fiber and the current density is 50min mA/cm2The distance between the cathode and anode electrode plates is 1 cm; and (3) after the electroplating processing is finished, washing with deionized water, and drying by blowing to obtain nickel-plated carbon fibers, wherein the carbon fibers after nickel plating are shown in figure 4.
(3) Fluorination of
And (3) soaking the nickel-plated carbon fiber processed in the step (2) in a fluorosilane ethanol solution with the mass fraction of 0.5%, treating for 20min, and drying at the temperature of 70 ℃ to obtain the super-hydrophobic super-oleophylic nickel-plated carbon fiber.
Example 3:
(1) pretreatment of
Removing the photoresist by adopting an acetone method, sequentially soaking the carbon fiber in 500mL of acetone and deionized water, and ultrasonically cleaning for 60min for 2 times; removing oil stains on the surface by adopting an acid-alkali solution, ultrasonically cleaning the carbon fiber after the glue is removed by sequentially using a 2mol/L NaOH solution and a 2mol/L HCl solution for 20min, and cleaning by using deionized water; then soaking the carbon fiber with the greasy dirt removed on the surface in a mixed aqueous solution of ammonium peroxodisulfate and sulfuric acid, wherein the concentration of the ammonium peroxodisulfate is 300g/L, the concentration of the sulfuric acid is 200ml/L, simultaneously carrying out ultrasonic cleaning for 20min, and then carrying out cleaning with deionized water; and finally, neutralizing for 20min by using NaOH with the mass fraction of 20%, and then washing by using deionized water.
(2) Electroplating of nickel
The components and concentrations of the plating solution are as follows: 300g/L of nickel sulfate, 100g/L of nickel chloride, 50g/L of boric acid and 0.5g/L of sodium dodecyl sulfate are mixed to prepare an aqueous solution. Cutting single-bundle pretreated carbon fiber into 6cm multiplied by 3cm, placing the carbon fiber as a cathode and an anode nickel plate with the area size not smaller than that of the cathode in parallel and symmetrically, connecting the nickel plate with a power supply through a lead, connecting the nickel plate with the positive electrode of the power supply,The carbon fiber is connected with the cathode of the power supply and then is put into the electroplating solution to start electroplating processing, and the product of the carbon fiber electroplating processing time and the current density is 400 min-mA/cm2The distance between the cathode and anode electrode plates is 5 cm; and (3) after the electroplating processing is finished, cleaning with deionized water, and drying by blowing to obtain nickel-plated carbon fibers, wherein the carbon fibers after nickel plating are shown in figure 5.
(3) Fluorination of
And (3) soaking the nickel-plated carbon fiber processed in the step (2) in a fluorosilane ethanol solution with the mass fraction of 2%, treating for 60min, and drying at the temperature of 80 ℃ to obtain the super-hydrophobic super-oleophylic nickel-plated carbon fiber.
Claims (1)
1. A preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber is characterized by comprising the following steps:
(1) pretreatment: removing the photoresist by adopting an acetone method, and sequentially soaking the carbon fiber in acetone and deionized water for ultrasonic cleaning for 2-3 times; removing oil stains on the surface by using acid-alkali liquor, and ultrasonically cleaning the carbon fiber after the glue is removed by using 0.5-2 mol/L NaOH solution and 0.5-2 mol/L HCl solution in sequence, and cleaning by using deionized water; then soaking the carbon fiber with the greasy dirt removed on the surface in a mixed aqueous solution of ammonium peroxodisulfate and sulfuric acid, wherein the concentration of the ammonium peroxodisulfate is 50-300 g/L, and the concentration of the sulfuric acid is 50-200 ml/L, simultaneously carrying out ultrasonic cleaning, and then cleaning with deionized water to coarsen the surface of the carbon fiber so that the surface of the carbon fiber presents a rough microstructure; finally, NaOH with the mass fraction of 5% -20% is utilized for neutralization, and then deionized water is used for cleaning, so that the pretreatment process is completed; the time for removing the photoresist by the acetone is not less than 30min, and the soaking time for soaking in the mixed solution of ammonium peroxydisulfate and sulfuric acid is not less than 10 min;
(2) electroplating nickel: the components and concentrations of the plating solution are as follows: 50 g/L-300 g/L of nickel sulfate, 10 g/L-100 g/L of nickel chloride, 5 g/L-50 g/L of boric acid and 0.01 g/L-0.5 g/L of sodium dodecyl sulfate, and mixing to prepare an aqueous solution; cutting single-beam pretreated carbon fiber as cathode, symmetrically placing the carbon fiber in parallel with anode nickel plate with area size not less than that of the cathode, and connecting with DC power supply via wiresConnecting a nickel plate with a positive electrode of a power supply and connecting a carbon fiber with a negative electrode of the power supply, then placing the nickel plate into electroplating solution to start electroplating processing, and cleaning and drying after the electroplating processing is finished to obtain nickel-plated carbon fiber; the product of the carbon fiber electroplating processing time and the current density is 50-400 min mA/cm2The distance between the cathode and anode electrode plates is 1-5 cm;
(3) fluorination: soaking the nickel-plated carbon fiber processed in the step (2) in a fluorosilane ethanol solution with the mass fraction of 0.5-2% for treatment for 20-60min, and then drying to obtain the super-hydrophobic super-oleophylic nickel-plated carbon fiber; the drying temperature is not higher than 90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010097501.1A CN111228858B (en) | 2020-02-17 | 2020-02-17 | Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010097501.1A CN111228858B (en) | 2020-02-17 | 2020-02-17 | Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111228858A CN111228858A (en) | 2020-06-05 |
| CN111228858B true CN111228858B (en) | 2021-06-08 |
Family
ID=70878229
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010097501.1A Active CN111228858B (en) | 2020-02-17 | 2020-02-17 | Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111228858B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112482024B (en) * | 2020-11-26 | 2022-09-23 | 南京信息工程大学 | Preparation method of copper-plated carbon fabric electromagnetic shielding material |
| CN112999698A (en) * | 2021-03-04 | 2021-06-22 | 中国石油大学(华东) | Ni for oil-water separation3S2Method for preparing nano-rod/stainless steel net material |
| CN113521884B (en) * | 2021-06-30 | 2022-11-22 | 中海油能源发展股份有限公司 | Cylindrical oil-water separation filter element, assembly, preparation method and application thereof |
| CN114622400A (en) * | 2022-04-12 | 2022-06-14 | 武汉纺织大学 | Surface modification method for enhancing oxidation resistance and electric heating performance of carbon fiber |
| CN116285346A (en) * | 2023-02-22 | 2023-06-23 | 江苏科技大学 | Nickel-plated carbon fiber-based electromagnetic shielding film and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009018463A3 (en) * | 2007-08-01 | 2009-06-04 | Donaldson Co Inc | Fluoropolymer fine fiber |
| CN103952732A (en) * | 2014-04-11 | 2014-07-30 | 华南理工大学 | Metal super-hydrophobic surface and preparation method thereof |
| CN103981547A (en) * | 2014-05-05 | 2014-08-13 | 深圳清华大学研究院 | Preparation method for super-hydrophobic metal surface |
| CN106987876A (en) * | 2017-03-03 | 2017-07-28 | 四川农业大学 | A kind of preparation method of super-hydrophobic/oleophylic water-oil separating Ni Cu composite deposite nethike embranes |
| JP2019108594A (en) * | 2017-12-19 | 2019-07-04 | 住友金属鉱山株式会社 | Method for removing the droplet of water phase included in organic phase |
| CN110755888A (en) * | 2019-11-29 | 2020-02-07 | 济南大学 | Preparation method of super-hydrophobic oleophylic material |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5212687A (en) * | 1975-07-19 | 1977-01-31 | Sumitomo Metal Ind Ltd | Process for recovering oil |
| CN100547018C (en) * | 2007-04-19 | 2009-10-07 | 北京理工大学 | A kind of ferrocene base full conjugate polyaromatic superhydraulic film and preparation method |
| US20130330501A1 (en) * | 2010-07-19 | 2013-12-12 | Joanna Aizenberg | Hierarchical structured surfaces to control wetting characteristics |
| CN102965720A (en) * | 2012-11-04 | 2013-03-13 | 大连理工大学 | Method for preparing aluminum-base super-amphiphobic surface |
-
2020
- 2020-02-17 CN CN202010097501.1A patent/CN111228858B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009018463A3 (en) * | 2007-08-01 | 2009-06-04 | Donaldson Co Inc | Fluoropolymer fine fiber |
| CN103952732A (en) * | 2014-04-11 | 2014-07-30 | 华南理工大学 | Metal super-hydrophobic surface and preparation method thereof |
| CN103981547A (en) * | 2014-05-05 | 2014-08-13 | 深圳清华大学研究院 | Preparation method for super-hydrophobic metal surface |
| CN106987876A (en) * | 2017-03-03 | 2017-07-28 | 四川农业大学 | A kind of preparation method of super-hydrophobic/oleophylic water-oil separating Ni Cu composite deposite nethike embranes |
| JP2019108594A (en) * | 2017-12-19 | 2019-07-04 | 住友金属鉱山株式会社 | Method for removing the droplet of water phase included in organic phase |
| CN110755888A (en) * | 2019-11-29 | 2020-02-07 | 济南大学 | Preparation method of super-hydrophobic oleophylic material |
Non-Patent Citations (3)
| Title |
|---|
| Fabrication of Superhydrophobic Surfaces on Stainless Steel Mesh Substrates via Electro-brush Flow Plating Technology;Longgang Wang等;《Elsevier Science》;20180423;第68卷;第232-236页 * |
| 基于电化学加工技术的极端润湿性表面制备及应用研究;刘子艾，宋金龙;《中国会议》;20171117;第639-648页 * |
| 碳纤维金属化镀镍的研究进展;叶伟等;《科技视界》;20150505;第13卷(第3期);第8-10页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111228858A (en) | 2020-06-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111228858B (en) | Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber | |
| CN105088749B (en) | A kind of graphene/cotton compliant conductive fabric and preparation method thereof | |
| CN103066314B (en) | Fabric morphological polymer battery and preparation method thereof | |
| CN110040820B (en) | Titanium-based tin antimony oxide electrode modified by titanium dioxide net structure and preparation method thereof | |
| CN103066287B (en) | A kind of processing method of vanadium cell carbon felt | |
| CN109873106B (en) | Preparation method of halloysite-bacterial cellulose composite diaphragm | |
| CN109326460A (en) | A kind of preparation method of di-iron trioxide/carbon cloth composite and flexible electrode | |
| CN102005504A (en) | Silicon wafer fine hair making method capable of improving solar cell conversion efficiency | |
| CN108538630A (en) | A kind of preparation method of biomass carbon/graphene flexible compound film | |
| CN101660264A (en) | Method for preparing polyimide/silver composite conductive fiber | |
| CN1436889A (en) | Production process of conductive fabric via plasma treatment | |
| CN110164709B (en) | Preparation method of fiber/graphene/carbon quantum dot/cobalt nickel sulfide flexible electrode material | |
| CN108597906A (en) | A kind of preparation method of fiber/graphene/copper sulfide flexible electrode material | |
| CN101591795A (en) | The pickler and the using method thereof that are used for carbon nanotubes in composite coating | |
| CN103280585A (en) | Preparation method of foamed nickel carrier palladium iridium electrode | |
| CN113445331A (en) | Dyeing method for improving dyeing performance of polyimide fibers | |
| CN112678924A (en) | Preparation method and application of hydrothermal modified graphite felt electrode applied to electro-Fenton system | |
| CN204991853U (en) | A super -hydrophobic porous flow field board for direct methanol fuel cell | |
| CN107871614A (en) | A kind of DSSC using eggshell film preparation is to electrode material and method | |
| CN107217491B (en) | The method of the modified chopped carbon fiber of polyaniline-coated | |
| CN114561663B (en) | NiFeCr composite hydroxide oxygen evolution material with nano-flake structure prepared by chemical oxidation method | |
| CN110136976B (en) | Preparation method of fiber/graphene/carbon quantum dot/FeOOF flexible electrode material | |
| CN113012946A (en) | Preparation method of phosphorus-doped NiCoB/graphene/fabric supercapacitor electrode material | |
| CN114622206A (en) | NH (hydrogen sulfide)2-MIL-101(Cr)/TiO2Composite photo-anode and preparation method and application thereof | |
| CN111128559B (en) | Preparation method of fabric-based metal/metal hydroxide flexible composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |