CN109821425B - Super-hydrophilic super-oleophobic metal net and preparation method thereof - Google Patents
Super-hydrophilic super-oleophobic metal net and preparation method thereof Download PDFInfo
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- CN109821425B CN109821425B CN201910183412.6A CN201910183412A CN109821425B CN 109821425 B CN109821425 B CN 109821425B CN 201910183412 A CN201910183412 A CN 201910183412A CN 109821425 B CN109821425 B CN 109821425B
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- 239000002184 metal Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000010410 layer Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 19
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 19
- 239000002344 surface layer Substances 0.000 claims abstract description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 13
- 239000010959 steel Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- LPUHOQKOQGQIKW-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpentan-1-one Chemical compound CCCC(C)(O)C(=O)C1=CC=CC=C1 LPUHOQKOQGQIKW-UHFFFAOYSA-N 0.000 claims description 3
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 231100001240 inorganic pollutant Toxicity 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 9
- 230000004907 flux Effects 0.000 abstract description 9
- 230000008929 regeneration Effects 0.000 abstract description 9
- 238000011069 regeneration method Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 238000011001 backwashing Methods 0.000 abstract description 5
- 238000012423 maintenance Methods 0.000 abstract description 5
- 230000003373 anti-fouling effect Effects 0.000 abstract description 4
- 239000003921 oil Substances 0.000 description 9
- 235000019198 oils Nutrition 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 235000019476 oil-water mixture Nutrition 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000010170 biological method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a super-hydrophilic super-oleophobic metal net and a preparation method thereof, wherein the super-hydrophilic super-oleophobic metal net comprises a metal net, the metal net comprises a plane net arranged on a top layer and four layers of woven nets arranged below the plane net in sequence, a metal oxide layer is arranged on the outer surface of the metal net, and a hydrophilic oleophobic surface layer is attached to the outer surface of the metal oxide layer. According to the invention, the metal oxide layer is arranged on the outer surface of the metal mesh, the hydrophilic oleophobic surface layer is attached to the outer surface of the metal oxide layer, the preparation process is simple, the time consumption is short, the cost is low, the prepared super-hydrophilic superoleophobic metal mesh is high in separation efficiency, large in membrane flux and strong in anti-fouling capability, has good chemical stability and mechanical stability, prolongs the service life, and meanwhile has the advantage of wider adaptability to water quality, the backwashing regeneration period is doubled, the membrane flux can be recovered by 100% after backwashing, the regeneration capability is good, the membrane maintenance and replacement cost is reduced, and the economic applicability is improved.
Description
Technical Field
The invention relates to the technical field of metal films, in particular to a super-hydrophilic super-oleophobic metal net and a preparation method thereof.
Background
At present, most of oil fields in China adopt a secondary oil recovery (or tertiary oil recovery) process, a large amount of oil field wastewater is generated after crude oil is dehydrated, in order to ensure a single well continuous high-yield and stable stratum structure, the oil-containing wastewater is subjected to advanced treatment, water is reinjected into the ground by a high-pressure pump after reaching the reinjection water standard, so that stratum energy is increased, extraction efficiency is improved, pollution is reduced, water resources are saved, and the oil-containing wastewater treatment mainly adopts an upward floating method, a biological method, a centrifugal separation method, a membrane treatment method and the like.
The membrane treatment method has the advantages of high efficiency, small equipment, less consumption, simple and convenient operation, easy realization of automatic control, easy industrial scale use and the like, is widely used in the treatment of oilfield produced water, and the effluent can be used as oilfield reinjection water, so that the method has huge social and economic benefits and wide application prospects. However, the metal film used in the film treatment method in the prior art has the following defects:
(1) The metal film has poor anti-pollution capability, the water quality of the effluent cannot meet the requirement, so that the film is frequently cleaned, the film regeneration capability is poor, and the film treatment use cost is higher;
(2) The membrane flux is gradually reduced along with the extension of time in the use process, the water yield is continuously reduced, the metal membrane is frequently replaced, and the cost is increased;
(3) The manufacturing process is complex, the time is long, the cost is high, and the stability of the obtained metal film is poor.
In view of this, there is an urgent need to improve the existing metal film and the manufacturing method thereof, simplify the manufacturing process, reduce the cost, and enable to obtain a metal film with good stability, and at the same time, increase the anti-contamination and film regeneration capabilities of the metal film, reduce the maintenance and replacement costs of the film, and improve the economic applicability.
Disclosure of Invention
The invention aims to solve the technical problems that the existing metal film and the manufacturing method thereof have the problems of complex manufacturing process, high cost, poor stability of the obtained metal film, poor pollution resistance and film regeneration capability of the metal film and high film maintenance and replacement cost.
In order to solve the technical problems, the technical scheme adopted by the invention is to provide the super-hydrophilic super-oleophobic metal net, wherein the metal net comprises a plane net arranged on the top layer and four layers of woven nets arranged below the plane net in sequence, the outer surface of the metal net is provided with a metal oxide layer, and the outer surface of the metal oxide layer is attached with a hydrophilic oleophobic surface layer.
In the above scheme, each layer of the woven net consists of two rows of wavy steel wires and one row of straight steel wires, and the two rows of wavy steel wires are oppositely staggered, so that a gap into which the straight steel wires can be inserted is formed in the middle of the woven net.
In the above scheme, the metal mesh is made of stainless steel.
In the above scheme, the pore diameter of the metal mesh is greater than or equal to 5 μm.
The invention also provides a preparation method of the super-hydrophilic super-oleophobic metal net, which comprises the following steps:
ultrasonically cleaning the metal net, removing organic and inorganic pollutants on the surface, and drying;
weigh a certain amount of FeCl 3 .6H 2 O, adding deionized water for dissolution, and sequentially adding strong acid and H 2 O 2 Preparing etching liquid;
weighing a certain amount of ethanol, methacryloyloxyethyl trimethyl ammonium chloride solution, a cross-linking agent and a photoinitiator to prepare a modified liquid;
immersing the dried metal net into the prepared etching liquid for 1-10 min, taking out, cleaning and drying;
immersing the etched metal net in the prepared modification liquid for 1-10 min, and taking out and drying;
and (3) placing the modified and dried metal net under an ultraviolet lamp for illumination for a period of time to obtain the super-hydrophilic super-oleophobic metal net.
In the scheme, the metal mesh is sequentially ultrasonically cleaned by deionized water, acetone, ethanol and deionized water.
In the above scheme, the crosslinking agent adopts trimethylolpropane triacrylate.
In the above scheme, the photoinitiator is 2-hydroxy-2-propyl propiophenone.
Compared with the prior art, the method has the advantages that the metal oxide layer is arranged on the outer surface of the metal mesh, the hydrophilic oleophobic surface layer is attached to the outer surface of the metal oxide layer, the preparation process is simple, the time consumption is short, the cost is low, the prepared super-hydrophilic super-oleophobic metal mesh is high in separation efficiency, large in membrane flux and high in anti-fouling capacity, has good chemical stability and mechanical stability, prolongs the service life, meanwhile has the advantage of wider adaptability to water quality, the backwashing regeneration period is doubled, the membrane flux can be recovered by 100%, the regeneration capacity is good, the membrane maintenance and replacement cost is reduced, and the economic applicability is improved.
Drawings
FIG. 1 is a schematic view of a metal mesh according to the present invention;
FIG. 2 is a schematic structural view of the super-hydrophilic super-oleophobic metal mesh of the invention;
FIG. 3 is an SEM image of the surface of an unmodified pre-expanded metal;
FIG. 4 is a schematic illustration of the contact angle of the unmodified pre-metal mesh with water;
FIG. 5 is an SEM image of the etched metal mesh surface of the present invention;
FIG. 6 is an SEM image of the surface of a super hydrophilic and super oleophobic metal mesh of the invention.
Detailed Description
The invention provides a super-hydrophilic super-oleophobic metal net and a preparation method thereof, which have the advantages of simple preparation process, short time consumption, low cost, high separation efficiency of the prepared super-hydrophilic super-oleophobic metal net, large membrane flux, strong anti-fouling capability, good chemical stability and mechanical stability, prolonged service life and wider adaptability to water quality. The invention is described in detail below with reference to the drawings and the detailed description.
As shown in fig. 1 and 2, the super-hydrophilic super-oleophobic metal mesh provided by the invention, the metal mesh 10 comprises a planar mesh arranged on the top layer and four layers of woven meshes arranged below the planar mesh in sequence, the outer surface of the metal mesh 10 is provided with a metal oxide layer 20, and a hydrophilic oleophobic surface layer 30 is attached to the outer surface of the metal oxide layer 20.
Further preferably, as shown in fig. 1, each layer of the woven mesh is composed of two rows of wavy steel wires and one row of straight steel wires, and the two rows of wavy steel wires are oppositely staggered, so that a gap into which the straight steel wires can be inserted is formed at the middle part of the woven mesh.
According to the invention, the metal oxide layer 20 can be formed on the surface of the metal net 10 by an oxidation method, the nano rough structure of the metal oxide has higher surface energy, water is very easy to infiltrate on the surface of the metal oxide, and the metal oxide can be hydrophilic and oleophobic, and in the state, water can pass through the net film, but oil cannot pass through the net film, so that oil-water separation of an oil-water mixture is realized. In order to increase the hydrophilic and oleophobic properties of the metal mesh 10, the oxidized metal mesh 10 may be immersed in a modifying liquid to attach hydrophilic substances to the outer periphery thereof and form a hydrophilic and oleophobic surface layer 30, thereby further increasing the hydrophilic and oleophobic effects.
The super-hydrophilic super-oleophobic metal net 10 has the advantages of high separation efficiency, high membrane flux, strong anti-fouling capability, good chemical stability and mechanical stability, prolonged service life, wider adaptability to water quality, doubled backwashing regeneration period, 100% recovery of membrane flux after backwashing, good regeneration capability, reduced membrane maintenance and replacement cost and improved economic applicability.
As shown in fig. 1, the metal mesh 10 of the present invention is a standard five-layer mesh structure, which is a novel filtering material formed by sequentially stacking five layers of stainless steel meshes and vacuum sintering, and the design mode is that the plane mesh forms a protective layer 11, and four layers of woven meshes form a filtering layer 12, a dispersing layer 13, a supporting framework layer 14 and a framework layer 15 from top to bottom.
Such a metal mesh 10 has the following advantages:
(1) The high-strength steel has extremely high mechanical strength and compressive strength, good processing, welding and assembling performances and convenient use;
(2) The filter layer 12 is arranged on the second layer, so that the filter layer is well protected and split, the filter precision can achieve uniform and consistent filter performance, and the filter layer is ensured to have high stability;
(3) The 316L material is selected, so that the corrosion resistance and the heat resistance are good, the filter can be used for filtering at the temperature of-200 ℃ to 480 ℃ and in an acid-base environment, and the application range is wide;
(4) The surface layer filtering structure with excellent countercurrent cleaning effect has excellent countercurrent cleaning effect, repeated use and long service life.
Further preferably, the metal mesh 10 is made of stainless steel, and the pore diameter of the metal mesh 10 is greater than or equal to 5 μm.
The invention also provides a preparation method of the super-hydrophilic super-oleophobic metal net 10, which comprises the following steps:
step one, carrying out ultrasonic cleaning on a metal net 10, removing organic and inorganic pollutants on the surface, and drying; specifically, the metal mesh 10 is sequentially ultrasonically cleaned by deionized water, acetone, ethanol and deionized water.
Step two, weighing a certain amount of FeCl 3 .6H 2 O, adding deionized water for dissolution, and sequentially adding strong acid and H 2 O 2 An etching liquid is prepared.
And thirdly, weighing a certain amount of ethanol, methacryloxyethyl trimethyl ammonium chloride solution, a cross-linking agent and a photoinitiator to prepare a modified solution, and obtaining the hydrophilic substance. Specifically, the crosslinking agent adopts trimethylolpropane triacrylate, and the photoinitiator adopts 2-hydroxy-2-propyl propiophenone.
Step four, as shown in fig. 5, the dried metal net 10 is immersed into the prepared etching liquid, soaked for 1-10 min, taken out, cleaned and dried; in this process, the metal oxide layer 20 is formed on the surface of the metal mesh 10, and the nano rough structure of the metal oxide has higher surface energy, so that water is very easy to infiltrate on the surface of the metal oxide layer, and the metal mesh has the characteristics of hydrophilicity and oleophobicity.
Step five, as shown in fig. 6, immersing the etched metal mesh 10 in the prepared modification liquid for 1-10 min, and taking out and drying; in this process, the surface of the metal mesh 10 is formed with a hydrophilic oleophobic surface layer 30, which increases the hydrophilic oleophobic property of the metal mesh 10.
And step six, the modified and dried metal net 10 is placed under an ultraviolet lamp for illumination for a period of time to obtain the super-hydrophilic super-oleophobic metal net 10, and the stability of the metal net 10 can be increased by adopting an ultraviolet curing mode, so that the metal net 10 has good chemical stability and mechanical stability, and the service life is prolonged.
As shown in FIG. 3, more water is attached to the surface of the common metal net, so that the metal net has poor hydrophilic and oleophobic properties, is unfavorable for separation of oil and water, and cannot meet the requirements on water yield and water quality. As shown in fig. 4, the contact angle of the metal mesh to water is about 94 °, which is unfavorable for water to pass through the metal mesh and reduces the water yield.
The super-hydrophilic super-oleophobic metal net 10 can be prepared through simple oxidation reaction and crosslinking reaction, and has the advantages of simple preparation process, short time consumption and low cost. As shown in fig. 5 and 6, the prepared super-hydrophilic super-oleophobic metal net film has high flux and higher surface energy, water is very easy to infiltrate on the surface of the super-hydrophilic super-oleophobic metal net film, and the super-hydrophilic super-oleophobic metal net film has the characteristics of hydrophilic and oleophobic, in the state, water can pass through the net film, and oil can not pass through the net film, so that oil-water separation of an oil-water mixture is realized, the hydrophilic and oleophobic characteristics of the metal net are increased, the oil-water separation efficiency is increased, and the requirement of water quality of effluent is met.
The present invention is not limited to the above-mentioned preferred embodiments, and any person who can learn the structural changes made under the teaching of the present invention can fall within the scope of the present invention if the present invention has the same or similar technical solutions.
Claims (5)
1. The preparation method of the super-hydrophilic super-oleophobic metal net is characterized in that the metal net comprises a plane net arranged on the top layer and four layers of woven nets arranged below the plane net in sequence, the outer surface of the metal net is provided with a metal oxide layer, and a hydrophilic oleophobic surface layer is attached to the outer surface of the metal oxide layer; the plane net and the woven net are both made of stainless steel wire nets, and are stacked together in sequence and sintered in vacuum, and the preparation method comprises the following steps:
ultrasonically cleaning the metal net, removing organic and inorganic pollutants on the surface, and drying;
weigh a certain amount of FeCl 3 ·6H 2 O, adding deionized water for dissolution, and sequentially adding strong acid and H 2 O 2 Preparing etching liquid;
weighing a certain amount of ethanol, methacryloyloxyethyl trimethyl ammonium chloride solution, a cross-linking agent and a photoinitiator to prepare a modified liquid;
immersing the dried metal net into the prepared etching liquid for 1-10 min, taking out, cleaning and drying;
immersing the etched metal net in the prepared modification liquid for 1-10 min, and taking out and drying;
placing the modified and dried metal net under an ultraviolet lamp for illumination for a period of time to obtain a super-hydrophilic super-oleophobic metal net;
the cross-linking agent adopts trimethylolpropane triacrylate, and the photoinitiator adopts 2-hydroxy-2-propyl propiophenone.
2. The method for preparing the super-hydrophilic and super-oleophobic metal net according to claim 1, wherein the metal net is sequentially subjected to ultrasonic cleaning by deionized water, acetone, ethanol and deionized water.
3. A super-hydrophilic super-oleophobic metal net is characterized in that the super-hydrophilic super-oleophobic metal net is prepared by the preparation method of claim 1.
4. A super hydrophilic and super oleophobic metal net according to claim 3, wherein each layer of said woven net is composed of two rows of wavy steel wires and one row of straight steel wires, said two rows of wavy steel wires being arranged in a staggered manner so that the middle portions thereof form gaps into which the straight steel wires are inserted.
5. A superhydrophilic superoleophobic metal mesh according to claim 3, wherein the metal mesh has a pore size of greater than or equal to 5 μm.
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| CN201910183412.6A CN109821425B (en) | 2019-03-12 | 2019-03-12 | Super-hydrophilic super-oleophobic metal net and preparation method thereof |
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| CN111228894A (en) * | 2020-03-11 | 2020-06-05 | 金碳环境科技（天津）有限公司 | Metal net for water treatment |
| CN114377435A (en) * | 2022-01-18 | 2022-04-22 | 中国石油大学(华东) | Preparation method of super-durable oil-water separation net |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105268326A (en) * | 2015-09-30 | 2016-01-27 | 西南交通大学 | Preparation of oil-water separation mesh membrane and surface wettability conversion method thereof |
| WO2018026328A1 (en) * | 2016-08-04 | 2018-02-08 | Nanyang Technological University | Multifunctional superhydrophilic and underwater superoleophobic activated glass derived from waste glass |
| CN109107226A (en) * | 2018-08-27 | 2019-01-01 | 大连理工大学 | A kind of metal mesh for oil-water separation preparation method that wetability is controllable |
| KR20190014712A (en) * | 2017-08-03 | 2019-02-13 | 한국과학기술연구원 | Oil-water separation structure, method for preparing the same, and oil-water separation method using the same |
| CN109381893A (en) * | 2017-08-03 | 2019-02-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of super hydrophilic oleophobic material, preparation method and application |
| CN209985222U (en) * | 2019-03-12 | 2020-01-24 | 浙江金龙自控设备有限公司 | Super-hydrophilic super-oleophobic metal net |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IN2014DN03394A (en) * | 2011-09-28 | 2015-06-05 | Univ King Abdullah Sci & Tech | |
| US9352258B2 (en) * | 2013-01-10 | 2016-05-31 | Massachusetts Institute Of Technology | Liquid collecting permeable structures |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105268326A (en) * | 2015-09-30 | 2016-01-27 | 西南交通大学 | Preparation of oil-water separation mesh membrane and surface wettability conversion method thereof |
| WO2018026328A1 (en) * | 2016-08-04 | 2018-02-08 | Nanyang Technological University | Multifunctional superhydrophilic and underwater superoleophobic activated glass derived from waste glass |
| KR20190014712A (en) * | 2017-08-03 | 2019-02-13 | 한국과학기술연구원 | Oil-water separation structure, method for preparing the same, and oil-water separation method using the same |
| CN109381893A (en) * | 2017-08-03 | 2019-02-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of super hydrophilic oleophobic material, preparation method and application |
| CN109107226A (en) * | 2018-08-27 | 2019-01-01 | 大连理工大学 | A kind of metal mesh for oil-water separation preparation method that wetability is controllable |
| CN209985222U (en) * | 2019-03-12 | 2020-01-24 | 浙江金龙自控设备有限公司 | Super-hydrophilic super-oleophobic metal net |
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