CN112813689B - Preparation method of oil-water separation fabric with super-hydrophilic-super-oleophobic property - Google Patents
Preparation method of oil-water separation fabric with super-hydrophilic-super-oleophobic property Download PDFInfo
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- CN112813689B CN112813689B CN202011557427.3A CN202011557427A CN112813689B CN 112813689 B CN112813689 B CN 112813689B CN 202011557427 A CN202011557427 A CN 202011557427A CN 112813689 B CN112813689 B CN 112813689B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 238000000926 separation method Methods 0.000 title claims abstract description 123
- 239000004744 fabric Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 59
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 29
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 29
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 29
- 239000000661 sodium alginate Substances 0.000 claims abstract description 29
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 29
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 229920001477 hydrophilic polymer Polymers 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 238000007654 immersion Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 35
- 239000004677 Nylon Substances 0.000 claims description 18
- 229920001778 nylon Polymers 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- 239000003208 petroleum Substances 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical group [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical group [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 3
- 229910001626 barium chloride Chemical group 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical group [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 229920002978 Vinylon Polymers 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- 239000008157 edible vegetable oil Substances 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 239000004328 sodium tetraborate Substances 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 229920004934 Dacron® Polymers 0.000 claims 1
- 239000004760 aramid Substances 0.000 claims 1
- 229920003235 aromatic polyamide Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 239000000017 hydrogel Substances 0.000 abstract description 9
- 238000004132 cross linking Methods 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 3
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- 239000012528 membrane Substances 0.000 description 56
- 235000019198 oils Nutrition 0.000 description 32
- 239000008367 deionised water Substances 0.000 description 24
- 229910021641 deionized water Inorganic materials 0.000 description 24
- 238000003756 stirring Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 238000002791 soaking Methods 0.000 description 12
- 238000002156 mixing Methods 0.000 description 9
- 235000019476 oil-water mixture Nutrition 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 239000002114 nanocomposite Substances 0.000 description 7
- 230000000717 retained effect Effects 0.000 description 7
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- 238000003760 magnetic stirring Methods 0.000 description 6
- 229920006231 aramid fiber Polymers 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229920004933 Terylene® Polymers 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
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- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010410 calcium alginate Nutrition 0.000 description 1
- 239000000648 calcium alginate Substances 0.000 description 1
- 229960002681 calcium alginate Drugs 0.000 description 1
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003305 oil spill Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
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- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
- D06M11/82—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
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- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
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Abstract
The invention relates to a preparation method of an oil-water separation fabric with super-hydrophilic-super-oleophobic properties. The method comprises the following steps: sequentially immersing the fabric into a hydrophilic polymer mixed solution, a curing solution and a precipitation solution, wherein the immersion time of each solution is as follows: taking out the fabric for 1-5 minutes, and drying the fabric for 0.5-1 hour at 45-55 ℃ to obtain the oil-water separation fabric with super-hydrophilic-super-oleophobic property; the hydrophilic polymer mixed solution is a mixed solution of a polyvinyl alcohol solution and a sodium alginate solution, and the volume ratio of the two mixed solutions is 10: 1-1: 10. The invention does not produce secondary pollution, is easy to clean, can be repeatedly used, does not need to modify and modify the fabric, only wraps the hydrogel hydrophilic material with interpenetrating networks on the fabric fiber in a simple crosslinking and curing mode, and has excellent water retention and oil stain resistance.
Description
Technical Field
The invention belongs to the technical field of chemical engineering and functional materials, and particularly relates to a preparation method and application of an oil-water separation fabric with super-hydrophilic-super-oleophobic properties.
Background
In recent years, with the rapid development of industry, the global demand for energy has increased to exacerbate the extraction of crude oil. Meanwhile, the increase of oil leakage and oil spill accidents has become one of the focuses of people. The traditional measures for dealing with large-scale oil leakage accidents include chemical dispersant degradation, in-situ combustion, vacuum oil absorption and the like. However, these methods are expensive, relatively inefficient, and even cause secondary pollution when they are put to practical use. More importantly, selective removal of oil from water is urgently required in order to recover valuable petroleum resources. Therefore, the development of an advanced material for selectively, efficiently and ecologically separating oil-water mixtures is urgent. In recent years, the development of specific wettability materials has been a hot spot of material research. Particularly, a particularly wettable material having diametrically opposite affinity for oil and water is considered as the most promising selective oil-water separation material. Specifically, there are two particular wettable materials suitable for oil-water separation, namely hydrophobic oleophilic materials and hydrophilic oleophobic materials.
The documents Ind.Eng.chem.Res,2014,53(17): 7141-7148; physical Chemistry Chemical Physics,2011,13(32): 14606-; separation and Purification Technology,2020,233: 116005; ind. Eng. chem. Res,2014,53(17): 7141-7148 reports sieves with super-hydrophobic and super-oleophilic properties for oil-water separation. Although these reported nethike webs can play a certain role in oil-water separation, they are high in production cost, complex in production process, harsh in treatment conditions and difficult to realize mass production, and due to the lipophilicity of these nethike webs, the nethike webs are particularly easy to be blocked by oil stains and difficult to clean in actual use, and further the oil-water separation effect is lost.
The document International Journal of Biological Macromolecules,2019,136:13-19 reports that a hydrophilic gel layer is coated on a metal net in a calcium ion cross-linked sodium alginate mode, and the underwater super-oleophobic metal net is formed by depositing the gel layer for multiple times, but a rough surface structure cannot be formed by using a hydrophilic polymer only, and the repeated use rate of the metal net is low due to poor adhesion of calcium alginate gel. In the method, toxic solvents such as tetrahydrofuran, acetone and the like are used in the preparation process, so that certain harm is caused to the health of operators, and the environment is polluted.
Disclosure of Invention
The invention aims to provide a preparation method of an oil-water separation fabric with super-hydrophilic-oleophobic properties, which is low in cost, simple and convenient, aiming at the defects in the prior art. According to the method, a mixed solution of polyvinyl alcohol and sodium alginate is adopted, a layer-by-layer self-assembly method is adopted, interpenetrating network hydrophilic gel is coated on fabric fibers, and inorganic hydrophilic particles are introduced in a mode of generating chemical precipitation on the surface, so that the roughness of the surface is increased, and the hydrophilicity is improved. According to the invention, modification and modification of the fabric are not required, and the hydrogel hydrophilic material with interpenetrating networks is wrapped on the fabric fibers only in a crosslinking and curing manner, so that the hydrogel has excellent water retention and oil stain resistance, and the oil-water separation fabric with super-hydrophilic-super-oleophobic properties is obtained. The invention does not produce secondary pollution, is easy to clean and can be repeatedly used.
The technical scheme of the invention is as follows:
a preparation method of an oil-water separation fabric with super-hydrophilic-super-oleophobic properties comprises the following steps:
(1) carrying out ultrasonic cleaning on 400-3000-mesh fabric, and then drying at room temperature;
the fabric is one of nylon, aramid fiber, vinylon and polyester fabric;
(2) sequentially immersing the fabric obtained in the step (1) into a hydrophilic polymer mixed solution, a curing solution and a precipitation solution, wherein the immersion time of each solution is as follows: and (3) taking out the fabric for 1-5 minutes, and drying the fabric for 0.5-1 hour at the temperature of 45-55 ℃ to obtain the oil-water separation fabric with super-hydrophilic-super-oleophobic property.
The hydrophilic polymer mixed solution is a mixed solution of a polyvinyl alcohol solution and a sodium alginate solution, and the mass concentration of the polyvinyl alcohol solution is 0.5-10%; the mass concentration of the sodium alginate solution is 0.5-10%; the volume ratio of the two solutions is 10: 1-1: 10.
The curing liquid contains a cross-linking agent A and a cross-linking agent B; the content of the cross-linking agent A in the curing liquid is 0.05-0.2 mol/L; the content of the cross-linking agent B is 0.1-0.2 mol/L.
The content of the precipitant is 0.05-0.5 mol/L.
The cross-linking agent A is boric acid or borax, and the cross-linking agent B is calcium chloride, copper sulfate, copper nitrate or barium chloride.
The precipitant is sodium carbonate, sodium hydroxide, sodium bicarbonate, potassium hydroxide or sodium sulfate.
The polymerization degree of the polyvinyl alcohol is 1700-2400.
The oil-water separation fabric with the super-hydrophilic-super-oleophobic property prepared by the method is applied to oil-water separation.
The oil is one or more of petroleum ether, kerosene, normal hexane, conduction oil, pump oil and edible oil.
The invention has the substantive characteristics that:
in the prior art, a hydrophilic layer is formed on a metal net and filter paper by crosslinking and curing sodium alginate, but the adhesion force is poor and the surface roughness is low, so the method for increasing the adhesion force and the roughness is provided and is applied to the fabric for oil-water separation; most of the prior methods for increasing the surface roughness are completed by blending and doping, and the invention increases the adhesive force of the coating by adding polyvinyl alcohol to form an interpenetrating network structure; the surface roughness is increased by further immersing the surface in a precipitation solution to form precipitates on the surface. In the preparation process, by using the proper volume ratio of the mixed solution of the polyvinyl alcohol and the sodium alginate, and by utilizing the good adhesive force of the polyvinyl alcohol, calcium ions, copper ions and the like can be introduced into the sodium alginate during crosslinking, and then the sodium alginate is impregnated by the precipitation solution, so that the ions can generate precipitates on the surface.
The invention has the beneficial effects that:
according to the oil-water separation fabric, inorganic particles and hydrogel are combined, interpenetrating network hydrogel and hydrophilic inorganic particles are coated on the meshes of the fabric net in a layer-by-layer self-assembly mode, the surface roughness and the hydrophilicity of the hydrogel are improved, and the oil-water separation effect is improved. Different from other organic-inorganic material coated fabrics, the interpenetrating network hydrogel is used as a hydrophilic organic matter, so that the water resistance and the adhesive force of the hydrogel are improved, and on the other hand, the inorganic particles are introduced in a chemical precipitation mode, so that the reaction time is short, and the precipitation can be quickly generated on the surface. The oil-water separation net membrane is hydrophilic in air, the net membrane is completely soaked by water, after the net membrane is completely soaked by the water, the water is filled into the micro-nano composite structure of the hydrogel coating layer, when an oil-water mixture contacts the oil-water separation net membrane, the water can smoothly permeate through pores, the oil is repelled by the water membrane on the surface of the oil-water separation net membrane and is retained above the oil-water separation net membrane, and the purpose of oil-water separation is achieved.
The method for preparing the oil-water separation fabric through layer-by-layer self-assembly has the advantages of simple operation, mild conditions, no need of using toxic solvents, no need of using expensive instruments and equipment and the like, and can realize large-scale production. The oil-water separation net film has a contact angle to water drops close to 0 degree in the air and a contact angle to oil drops larger than 150 degrees underwater, can be used for oil-water separation, and has high separation efficiency and good cyclic usability.
Drawings
FIG. 1 is a scanning electron micrograph of an oil-water separating fabric prepared in example 1 of the present invention;
FIG. 2 is a photograph showing the change in contact angle of water drops in the air of the oil-water separating fabric prepared in example 1 of the present invention, the four graphs from left to right being 0s, 1s, 1.5s and 1.8s, respectively, during the dropping of the water drops;
FIG. 3 is a schematic diagram of the super-oleophobic property of the oil-water separation fabric prepared in example 1 of the invention in water, wherein four diagrams from left to right are photographs of 0s, 1s, 4s and 5s in the oil dropping process respectively;
FIG. 4 is a photograph showing an underwater oil contact angle of the oil-water separating fabric prepared in example 1 of the present invention;
FIG. 5 is a photograph showing an experimental apparatus and an experimental effect of the oil-water separating fabric prepared in example 1 of the present invention, applied to oil-water separation;
FIG. 6 is a graph showing the relationship between the number of times of oil-water separation cycle and the separation efficiency when the oil-water separation fabric prepared in example 1 of the present invention is used for oil-water separation.
Detailed Description
Example 1.
(1) A1000 mesh (15 μm pore diameter) nylon net (5 cm. times.5 cm) was cleaned and dried at room temperature.
(2) A250 mL single-neck bottle is placed in a 95 ℃ oil bath kettle, 2.5g of polyvinyl alcohol (with the polymerization degree of 1700) and 150mL of deionized water (150g) are added into the single-neck bottle, and the mixture is stirred and dissolved for 2 hours at the temperature of 95 ℃ to obtain a colorless and transparent polyvinyl alcohol solution.
(3) 1g of sodium alginate and 150mL of deionized water (150g) are added into a 250mL single-neck flask at room temperature, and dissolved for 2h under stirring to obtain a light yellow transparent sodium alginate solution.
(4) And (3) adding 60mL of the solution obtained in the step (2) into a 100mL beaker, adding 40mL of the solution obtained in the step (3) into the 100mL beaker, and uniformly mixing to obtain 100mL of a mixed solution of the polyvinyl alcohol and the sodium alginate.
(5) 0.62g of boric acid (i.e., 0.01mol) and 2.11g of calcium chloride (i.e., 0.02mol) were added to a 100mL beaker, and then 100mL of deionized water was added thereto, followed by stirring at room temperature for 30min to obtain a solidified solution.
(6) 2.05g (i.e., 0.02mol) of sodium carbonate was added to a 100mL beaker, followed by 100mL of deionized water, and stirred at room temperature for 30min to obtain a precipitate.
(7) And (3) sequentially soaking the nylon net dried in the step (1) in the solutions obtained in the step (4), the step (5) and the step (6) for 3 minutes, taking out the nylon net, and drying the nylon net in a 50 ℃ oven for 1 hour to obtain the oil-water separation fabric, wherein a layer of rough structure is arranged on the surface of the net wire as shown in figure 1.
(8) By Germany
The contact angle was measured by a DSA30 contact angle measuring apparatus from the company, and the size of the water drop and oil drop taken during the measurement was 4. mu.L. A4 μ L drop of water was dropped onto the superhydrophilic-superoleophobic fabric of this example in air, and the contact angle as a function of time is shown in FIG. 2, and the four graphs from left to right are photographs of the dropping process of the drop of water at 0s, 1s, 1.5s and 1.8s, respectively. As can be seen from FIG. 2, the water contact angle becomes 0 ℃ within 2s, indicating thatThe fabric has super-hydrophilic properties. In water, 4. mu.L of dichloroethane was dropped on the superhydrophilic-superoleophobic fabric of this example, and the contact angle as a function of time is shown in FIG. 3, and the four graphs from left to right are photographs of the dropping process of the droplets at 0s, 1s, 4s and 5s, respectively. As can be seen from FIG. 3, the oil-water separation net has super-oleophobic property in water. The contact angle of the surface of the oil-water separation net obtained in the step (7) with 4. mu.L of dichloroethane was measured under water at 156.7 ° (as shown in FIG. 4).
(9) An oil-water separation experiment was performed using the experimental apparatus shown in fig. 5 (1: separated oil; 2: oil-water separation mesh membrane completely soaked with water; 3: separated water). Firstly, completely infiltrating the obtained oil-water separation net membrane 2 with water (the complete infiltration is that all parts of the oil-water separation net membrane 2 are contacted with water, for example, the oil-water separation net membrane 2 is immediately taken out after being immersed into water; the following embodiment is the same), then clamping the net membrane 2 in the middle of a separation device, pouring a mixture of petroleum ether and water (the volume ratio is 1:1, magnetic stirring is carried out for 20 minutes) onto the oil-water separation net membrane, when the net membrane is completely infiltrated with water, filling the water into a micro-nano composite structure on the surface of a net wire, and when the oil-water mixture is contacted with the oil-water separation net membrane, enabling the water to quickly penetrate through the oil-water separation net membrane to obtain separated water 3; meanwhile, petroleum ether is repelled by a water film on the surface of the oil-water separation net film and is retained above the oil-water separation net film to obtain separated oil 1, so that the purpose of oil-water separation is realized.
(10) The experimental apparatus shown in fig. 5 was used to test the recycling effect of the oil-water separating fabric. Mixing petroleum ether and water according to the volume ratio of 1:1, weighing the water before mixing and recording the weight of the water as M0Pouring the mixed solution on the oil-water separation net, and enabling the water to pass through the oil-water separation net to obtain separated water, wherein the weight of the weighed water is recorded as MSThe calculation formula of the oil-water separation efficiency is as follows: efficiency of oil-water separation (M)S/M0) X 100%, repeating the operation and testing the recycling effect. As can be seen from FIG. 6, the separation efficiency of the oil-water separation fabric reaches more than 99%, and even after 40 cycles, the separation efficiency can still be maintained at more than 98%, indicating that the oil-water separation fabric has good recyclability.
Example 2.
(1) Cleaning a 400-mesh (38 μm-pore diameter) nylon net (5 cm. times.5 cm), and drying at room temperature;
(2) placing a 250mL single-neck bottle into a 95 ℃ oil bath pot, adding 1.5g of polyvinyl alcohol (with the polymerization degree of 1700) and 150mL of deionized water (150g) into the single-neck bottle, and stirring and dissolving for 2 hours at the temperature of 95 ℃ to obtain a colorless and transparent polyvinyl alcohol solution;
(3) at room temperature, adding 0.75g of sodium alginate and 150mL of deionized water (150g) into a 250mL single-mouth bottle, and stirring and dissolving for 2 hours to obtain a light yellow transparent sodium alginate solution;
(4) adding 50mL of the solution obtained in the step (2) into a 100mL beaker, adding 50mL of the solution obtained in the step (3) into the 100mL beaker, and uniformly mixing to obtain 100mL of a mixed solution of polyvinyl alcohol and sodium alginate;
(5) 0.62g of boric acid and 1.59g of copper sulfate were added to a 100mL beaker, followed by addition of 100mL of deionized water, and stirred at room temperature for 30min to obtain a solidified solution.
(6) 0.4g of sodium hydroxide is added into a 100mL beaker, then 100mL of deionized water is added, and the mixture is stirred for 30min at room temperature to obtain a precipitate.
(7) And (3) soaking the nylon net dried in the step (1) in the solutions in the step (4), the step (5) and the step (6) for 3 minutes in sequence, taking out the nylon net, and drying the nylon net in a 50 ℃ oven for 1 hour to obtain the prepared oil-water separation fabric.
(8) An oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. Firstly, completely soaking the obtained oil-water separation net membrane with water (the complete soaking is that all parts of the oil-water separation net membrane are contacted with water, for example, the oil-water separation net membrane is taken out immediately after being immersed into water; the following embodiment is the same), then clamping the net membrane in the middle of a separation device, pouring a mixture of kerosene and water (the volume ratio is 1:1, magnetic stirring is carried out for 20 minutes) on the oil-water separation net membrane, when the net membrane is completely soaked with water, filling the water into a micro-nano composite structure on the surface of the net wire, and when the oil-water mixture is contacted with the oil-water separation net membrane, enabling the water to quickly penetrate through the oil-water separation net membrane to obtain separated water; meanwhile, the kerosene is repelled by a water film on the surface of the oil-water separation net film and is retained above the oil-water separation net film to obtain separated oil, so that the purpose of oil-water separation is realized.
Example 3.
(1) Cleaning a 400-mesh (aperture is 38 μm) terylene net (5 cm multiplied by 5 cm), and drying at room temperature;
(2) placing a 250mL single-neck bottle into a 95 ℃ oil bath pot, adding 3g of polyvinyl alcohol (with the polymerization degree of 2400) and 150mL of deionized water (150g) into the single-neck bottle, and stirring and dissolving for 2 hours at the temperature of 95 ℃ to obtain a colorless and transparent polyvinyl alcohol solution;
(3) at room temperature, adding 2g of sodium alginate and 150mL of deionized water (150g) into a 250mL single-mouth bottle, and stirring to dissolve for 2 hours to obtain a light yellow transparent sodium alginate solution;
(4) adding 40mL of the solution obtained in the step (2) into a 100mL beaker, adding 60mL of the solution obtained in the step (3) into the 100mL beaker, and uniformly mixing to obtain 100mL of a mixed solution of polyvinyl alcohol and sodium alginate;
(5) 0.62g of boric acid and 2.08g of barium chloride were added to a 100mL beaker, and then 100mL of deionized water was added thereto, followed by stirring at room temperature for 30min to obtain a solidified liquid.
(6) 2.42g of sodium sulfate was added to a 100mL beaker, followed by 100mL of deionized water, and the mixture was stirred at room temperature for 30min to obtain a precipitate.
(7) And (3) soaking the terylene net dried in the step (1) in the solutions obtained in the steps (4), (5) and (6) for 3 minutes in sequence, taking out the terylene net, and drying the terylene net in a 50 ℃ oven for 1 hour to obtain the oil-water separation fabric.
(8) An oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. Firstly, completely infiltrating the obtained oil-water separation net membrane with water (the complete infiltration is that all parts of the oil-water separation net membrane are contacted with water, for example, the oil-water separation net membrane is immediately taken out after being immersed into water; the following embodiment is the same), then clamping the net membrane in the middle of a separation device, pouring a mixture of heat conduction oil and water (the volume ratio is 1:1, magnetic stirring is carried out for 20 minutes) onto the oil-water separation net membrane, when the net membrane is completely infiltrated with water, filling the water into a micro-nano composite structure on the surface of the net wire, and when the oil-water mixture is contacted with the oil-water separation net membrane, enabling the water to quickly penetrate through the oil-water separation net membrane to obtain separated water; meanwhile, the heat conduction oil is repelled by a water film on the surface of the oil-water separation net film and is retained above the oil-water separation net film to obtain separated oil, so that the purpose of oil-water separation is realized.
Example 4.
(1) Cleaning a 2000-mesh (6.5 μm-pore diameter) nylon net (5 cm. times.5 cm), and drying at room temperature;
(2) placing a 250mL single-neck bottle into a 95 ℃ oil bath pot, adding 1g of polyvinyl alcohol (polymerization degree 2000) and 150mL of deionized water (150g) into the single-neck bottle, and stirring and dissolving for 2 hours at 95 ℃ to obtain a colorless and transparent polyvinyl alcohol solution;
(3) at room temperature, adding 3g of sodium alginate and 150mL of deionized water (150g) into a 250mL single-mouth bottle, and stirring to dissolve for 2 hours to obtain a light yellow transparent sodium alginate solution;
(4) adding 50mL of the solution obtained in the step (2) into a 100mL beaker, adding 50mL of the solution obtained in the step (3) into the 100mL beaker, and uniformly mixing to obtain 100mL of a mixed solution of polyvinyl alcohol and sodium alginate;
(5) 0.62g of boric acid and 1.59g of copper sulfate were added to a 100mL beaker, followed by addition of 100mL of deionized water, and stirred at room temperature for 30min to obtain a solidified solution.
(6) 1.56g of potassium hydroxide is added into a 100mL beaker, then 100mL of deionized water is added, and the mixture is stirred for 30min at room temperature to obtain a precipitate.
(7) And (3) soaking the nylon net dried in the step (1) in the solutions in the step (4), the step (5) and the step (6) for 3 minutes in sequence, taking out the nylon net, and drying the nylon net in a 50 ℃ oven for 1 hour to obtain the prepared oil-water separation fabric.
(8) An oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. Firstly, completely soaking the obtained oil-water separation net membrane with water (the complete soaking is that all parts of the oil-water separation net membrane are contacted with water, for example, the oil-water separation net membrane is taken out immediately after being immersed into water; the following embodiment is the same), then clamping the net membrane in the middle of a separation device, pouring a mixture of pump oil and water (the volume ratio is 1:1, magnetic stirring is carried out for 20 minutes) on the oil-water separation net membrane, when the net membrane is completely soaked with water, filling water into a micro-nano composite structure on the surface of the net wire, and when the oil-water mixture is contacted with the oil-water separation net membrane, enabling water to quickly penetrate through the oil-water separation net membrane to obtain separated water; meanwhile, the pump oil is repelled by the water film on the surface of the oil-water separation net film and is retained above the oil-water separation net film to obtain the separated oil, thereby realizing the purpose of oil-water separation.
Example 5.
(1) Cleaning a nylon net (5 cm multiplied by 5 cm) with 3000 meshes (the aperture is 5 mu m), and drying at room temperature;
(2) placing a 250mL single-neck bottle into a 95 ℃ oil bath pot, adding 2.5g of polyvinyl alcohol (with the polymerization degree of 1700) and 150mL of deionized water (with the polymerization degree of 150g) into the single-neck bottle, and stirring and dissolving for 2 hours at the temperature of 95 ℃ to obtain a colorless and transparent polyvinyl alcohol solution;
(3) at room temperature, adding 2.5g of sodium alginate and 150mL of deionized water (150g) into a 250mL single-mouth bottle, and stirring to dissolve for 2 hours to obtain a light yellow transparent sodium alginate solution;
(4) adding 70mL of the solution obtained in the step (2) into a 100mL beaker, adding 30mL of the solution obtained in the step (3) into the 100mL beaker, and uniformly mixing to obtain 100mL of a mixed solution of polyvinyl alcohol and sodium alginate;
(5) 0.62g of boric acid and 1.11g of calcium chloride were added to a 100mL beaker, followed by addition of 100mL of deionized water, and stirred at room temperature for 30min to obtain a solidified solution.
(6) 1.4g of sodium hydroxide is added into a 100mL beaker, then 100mL of deionized water is added, and the mixture is stirred for 30min at room temperature to obtain a precipitate.
(7) And (3) soaking the nylon net dried in the step (1) in the solutions in the step (4), the step (5) and the step (6) for 5 minutes in sequence, taking out the nylon net, and drying the nylon net in a 50 ℃ oven for 1 hour to obtain the prepared oil-water separation fabric.
(8) An oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. Firstly, completely infiltrating the obtained oil-water separation net membrane with water (the complete infiltration is that all parts of the oil-water separation net membrane are contacted with water, for example, the oil-water separation net membrane is immediately taken out after being immersed into water; the following embodiment is the same), then clamping the net membrane in the middle of a separation device, pouring a mixture of petroleum ether and water (the volume ratio is 1:1, magnetic stirring is carried out for 20 minutes) on the oil-water separation net membrane, when the net membrane is completely infiltrated with water, filling the water into a micro-nano composite structure on the surface of the net wire, and when the oil-water mixture is contacted with the oil-water separation net membrane, enabling the water to quickly penetrate through the oil-water separation net membrane to obtain the separated water; meanwhile, petroleum ether is repelled by a water film on the surface of the oil-water separation net film and is retained above the oil-water separation net film to obtain separated oil, so that the purpose of oil-water separation is realized.
Example 6.
(1) Cleaning a 400-mesh (38-micron aperture) aramid fiber net (5 cm multiplied by 5 cm), and drying at room temperature;
(2) placing a 250mL single-neck bottle into a 95 ℃ oil bath pot, adding 1.5g of polyvinyl alcohol (polymerization degree 2000) and 150mL of deionized water (150g) into the single-neck bottle, and stirring and dissolving for 2 hours at 95 ℃ to obtain a colorless and transparent polyvinyl alcohol solution;
(3) at room temperature, adding 2.5g of sodium alginate and 150mL of deionized water (150g) into a 250mL single-mouth bottle, and stirring to dissolve for 2 hours to obtain a light yellow transparent sodium alginate solution;
(4) adding 50mL of the solution obtained in the step (2) into a 100mL beaker, adding 50mL of the solution obtained in the step (3) into the 100mL beaker, and uniformly mixing to obtain 100mL of a mixed solution of polyvinyl alcohol and sodium alginate;
(5) 0.62g of boric acid and 1.87g of copper nitrate were added to a 100mL beaker, followed by addition of 100mL of deionized water, and stirred at room temperature for 30min to obtain a solidified solution.
(6) 0.4g of sodium hydroxide is added into a 100mL beaker, then 100mL of deionized water is added, and the mixture is stirred for 30min at room temperature to obtain a precipitate.
(7) And (3) soaking the aramid fiber net dried in the step (1) in the solutions in the step (4), the step (5) and the step (6) for 3 minutes in sequence, taking out the aramid fiber net, and drying the aramid fiber net in a 50-DEG C oven for 1 hour to obtain the prepared oil-water separation fabric.
(8) An oil-water separation experiment was performed using the experimental apparatus shown in fig. 5. Firstly, completely soaking the obtained oil-water separation net membrane with water (the complete soaking is that all parts of the oil-water separation net membrane are contacted with water, for example, the oil-water separation net membrane is taken out immediately after being immersed into water. the following embodiment is the same), then clamping the net membrane in the middle of a separation device, pouring a mixture of cyclohexane and water (the volume ratio is 1:1, magnetic stirring is carried out for 20 minutes) on the oil-water separation net membrane, when the net membrane is completely soaked with water, filling the water into a micro-nano composite structure on the surface of the net wire, and when the oil-water mixture is contacted with the oil-water separation net membrane, enabling the water to quickly penetrate through the oil-water separation net membrane to obtain separated water; meanwhile, cyclohexane is repelled by a water film on the surface of the oil-water separation net film and is retained above the oil-water separation net film to obtain separated oil, so that the purpose of oil-water separation is realized.
The invention is not the best known technology.
Claims (4)
1. A method for preparing an oil-water separation fabric with super-hydrophilic-super-oleophobic properties is characterized by comprising the following steps:
(1) carrying out ultrasonic cleaning on the fabric, and then drying at room temperature;
(2) sequentially immersing the fabric obtained in the step (1) into a hydrophilic polymer mixed solution, a curing solution and a precipitation solution, wherein the immersion time of each solution is as follows: taking out the fabric for 1-5 minutes, and drying the fabric for 0.5-1 hour at the temperature of 45-55 ℃ to obtain the oil-water separation fabric with super-hydrophilic-super-oleophobic properties;
the hydrophilic polymer mixed solution is a mixed solution of a polyvinyl alcohol solution and a sodium alginate solution, and the mass concentration of the polyvinyl alcohol solution is 0.5-10%; the mass concentration of the sodium alginate solution is 0.5-10%; the volume ratio of the two solutions is 10: 1-1: 10;
the curing liquid contains a cross-linking agent A and a cross-linking agent B; the content of the cross-linking agent A in the curing liquid is 0.05-0.2 mol/L; the content of the cross-linking agent B is 0.1-0.2 mol/L;
the content of the precipitant in the precipitation solution is 0.05-0.5 mol/L;
the cross-linking agent A is boric acid or borax, and the cross-linking agent B is calcium chloride, copper sulfate, copper nitrate or barium chloride;
the precipitant is sodium carbonate, sodium hydroxide, sodium bicarbonate, potassium hydroxide or sodium sulfate.
2. The method for preparing the oil-water separation fabric with super hydrophilic-super oleophobic property as claimed in claim 1, characterized in that the fabric is one of nylon, aramid, vinylon and dacron; the mesh number of the fabric is 400-3000 meshes.
3. The method for preparing the oil-water separation fabric with the super-hydrophilic-super-oleophobic property as claimed in claim 1, wherein the polymerization degree of the polyvinyl alcohol is 1700-2400.
4. Use of a superhydrophilic-superoleophobic fabric made according to the method described in claim 1 for oil-water separation;
the oil is one or more of petroleum ether, kerosene, normal hexane, conduction oil, pump oil and edible oil.
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| CN110541304A (en) * | 2019-08-02 | 2019-12-06 | 江苏涌金化纤有限公司 | preparation method of single-sided hydrophilic modified polyester fabric |
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