CN105268326A - Preparation of oil-water separation mesh membrane and surface wettability conversion method thereof - Google Patents
Preparation of oil-water separation mesh membrane and surface wettability conversion method thereof Download PDFInfo
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- CN105268326A CN105268326A CN201510642408.3A CN201510642408A CN105268326A CN 105268326 A CN105268326 A CN 105268326A CN 201510642408 A CN201510642408 A CN 201510642408A CN 105268326 A CN105268326 A CN 105268326A
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Abstract
Preparation of an oil-water separation mesh membrane and its surface wettability conversion method are disclosed. The preparation of the separation mesh membrane comprises the following steps: A, a micro-nano structure is constructed on the surface of a metal mesh membrane by an oxidation method; B, the metal mesh membrane with the nicro-nano structure on the surface in the step A is put into an electric furnace to undergo thermo-oxidative treatment in the air atmosphere at the thermo-oxidative treatment temperature of 180-300 DEG C for 3-20 min; and a product is taken out of the electric furnace to obtain a superhydrophilic oleophobic mesh membrane; and C, the superhydrophilic oleophobic mesh membrane prepared in the step B is immersed in an ethanol solution of long-chain alkanoic acid or long-chain alkyl sulfhydryl at room temperature for 1-30 min, the product is taken out of the solution and then washed with ethanol, and finally the product is dried in a drying oven of 50-70 DEG C for 8-20 min so as to obtain the superhydrophobic oleophylic mesh membrane. The superhydrophobic oleophylic mesh membrane undergoes the treatment in the step B and the superhydrophilic oleophobic mesh membrane undergoes treatment in the step C so as to change surface wettability of the mesh membrane. The method is simple to operate, and the prepared mesh membrane material has good separation efficiency. In addition, surface wettability of the mesh membrane can be changed through simple operations.
Description
Technical field
The invention belongs to the preparation field of the pellicle for separating of technique, be specifically related to preparation and the surface wettability method of converting thereof of the reversible oil-water separation mesh film of a kind of surface wettability.
Background technology
It is many convenient and comfortable that the quickening of expanding economy and modernization brings to human lives, also brings the problems such as the energy shortage become increasingly conspicuous and environmental pollution simultaneously.As oil pollution water, the discharge etc. of crude oil leakage and oily waste water causes serious harm to environment.At present, oily water separation technique is used widely in multiple fields such as petrochemical industry, sewage disposal, food engineerings.But the difference of the factors such as organism kinds contained in oil mixing with water state, profit content and oil-water mixture, adds the difficulty of water-oil separating.At present, oily water separation technique mainly contains: gravitational separation process, electricity de-partition method, centrifugal separation, method of chemical treatment and coarse separation method.The application that but efficiency is lower, comparatively large and caused by chemical reagent the secondary pollution etc. of energy consumption limits above-mentioned facture.Therefore, how effectively to realize the water-oil separating of oil water mixture and reusablely become problem urgently to be resolved hurrily.
Because the surface tension between water and oil exists larger difference, select the oil material different with water logging lubricant nature, can selective oil phase in oil water mixture and aqueous phase be adsorbed and excretion, realize being separated with water oily in oil water mixture.By the acting in conjunction of surface microstructure and chemical composition, can obtain having special infiltrating surface, the preparation on special wellability surface is mainly concerned with constructing and surface chemical modification of surperficial micro-nano roughness.The wellability on reinforcing material surface effectively can improve the efficiency of material water-oil separating.
Based on the controllable immersing of material surface, a lot of super-hydrophobic oleophylic class separate mesh membrane material is produced out and for water-oil separating.But, due to the difference of water and oil density, the viscosity differences of different oils, and the factor such as in different oil water mixture oil-water ratio is uncertain, above-mentioned parting material is caused still to there is following shortcoming: one is for the little oils of density ratio water, oil swims on water face, water tends to be formed between oil and super-hydrophobic oleophylic parting material superficial layer stop, thus reduces the infiltration of oils.Two is for the larger oils of ratio of viscosities, fiber web material surface can be adhered to when the web structure through super-hydrophobic oleophylic class parting material, destroy material surface structure and reduce the wellability of material surface, thus reducing its separative efficiency, and shortening the service life being separated nethike embrane.Three is for the higher oil water mixture of oil content ratio, and super-hydrophobic oleophylic class parting material is selected to be separated the separative efficiency that oils greatly reduces material.
Summary of the invention
First goal of the invention of the present invention is to provide a kind of preparation method of oil-water separation mesh film.The method can prepare super hydrophilic oleophobic nethike embrane and super-hydrophobic oleophylic nethike embrane, and preparation process is simple, and consuming time short, cost is low, and the oil-water separating net membrane material separative efficiency of preparation is good, has good chemical stability and mechanical stability, long service life.
The present invention realizes the technical scheme that its first goal of the invention takes: a kind of preparation method of oil-water separation mesh film, comprises the following steps:
A, oxidizing process are at metal nethike embrane surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the metal nethike embrane of micro-nano structure is placed in electric furnace by the surface of preparing in steps A, thermal oxidation in air atmosphere, the time of thermal oxidation is 3 ~ 20min, and the temperature of thermal oxidation is 180 ~ 300 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: the super hydrophilic oleophobic nethike embrane prepared by step B immerses in the ethanolic solution of long-chain alkanoic acid or chain alkyl mercaptan, take out after soaking 1 ~ 30min under room temperature, with after alcohol flushing 1 ~ 3 time in 50 ~ 70 DEG C of oven drying 8 ~ 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
The principle of this technical scheme is:
Steps A is by oxidizing process at metal nethike embrane surface construction micro-nano structure, and the burning of metal retinal surface is metal oxide by thermal oxidation by step B.The metal oxide nano coarse structure of metal retinal surface has higher surface energy, and water electrode easily infiltrates on its surface, presents the characteristic of hydrophilic oleophobic; Under this state, water can pass through nethike embrane, and oils is not by cover net film, thus realizes the water-oil separating of oil water mixture.
The super hydrophilic oleophobic nethike embrane of step C to above-mentioned preparation carries out simple wet-chemical treatment, is immersed by the nethike embrane of above-mentioned preparation in the ethanolic solution of long-chain alkanoic acid or chain alkyl mercaptan, reaction certain hour, and for metallic copper, reaction equation is:
Long-chain alkanoic acid: 2CH
3(CH
2)
ncOOH+CuO → Cu [CH
3(CH
2)
ncOO]
2+ H
2o
Long chain mercaptans: 2CH
3(CH
2)
nsH+CuO → Cu [CH
3(CH
2)
ns]
2+ H
2o
In reaction, the alkanoic acid of long-chain and the effect of alkyl hydrosulfide form one deck chain alkyl on the coarse web structure surface of above-mentioned preparation, thus the surface energy of degradation retinal surface micro-nano structure, promote that nethike embrane is to super-hydrophobic oleophylic state transfer.
Compared with prior art, the beneficial effect of the technical program is:
One, the method can prepare super hydrophilic oleophobic nethike embrane and super-hydrophobic oleophylic nethike embrane by simple thermal oxidation and wet chemistry method process, preparation process is simple, consuming time short, cost is low, and the oil-water separating net membrane material separative efficiency of preparation is good, there is good chemical stability and mechanical stability, long service life.
Two, the oil-water separation mesh film surface wettability of preparation can fast transition and controlled, can according to the density of oil in oil water mixture, viscosity, the features such as mixed proportion, control targetedly be separated the wellability of nethike embrane or change the wellability of nethike embrane fast, thus realize being separated fast and efficiently oil water mixture.
Further, in A of the present invention step oxidizing process for construct micro-nano structure by dithionate oxidized metal nethike embrane in alkaline medium.
Further, sodium hydroxide solution or the potassium hydroxide solution of alkaline medium of the present invention to be concentration be 0.5 ~ 7.5mol/L.
Further again, two potassium sulfate solutions of dithionate of the present invention to be concentration be 0.01 ~ 0.5mol/L, one or more mixed solution of two metabisulfite solutions or two ammonium sulfates.
Micro-nano structure reaction condition is constructed simple by above-mentioned oxidizing process, at room temperature can carry out, and micro-nano structure to construct speed fast, consuming time short, the micro-nano structure constructed is evenly distributed at retinal surface, ensure that the homogeneity of fiber web material performance, and micro-nano structure has better chemical stability and structural stability, utilize the service life of improving nethike embrane.
Further, metal nethike embrane of the present invention is 150 ~ 400 object copper mesh, stainless (steel) wire, titanium net or aluminium net.
In oil water mixture, the droplet-like that oil is several microns to hundreds of microns with diameter is distributed in water, nethike embrane order number is larger, retinal surface aperture is less, the separating effect of oil water mixture is improved, but water is increased by the difficulty in aperture, net membrane separation efficiency reduces, and nethike embrane order number is less, retinal surface aperture is larger, oil droplet in oil water mixture easily penetrates nethike embrane, the separating effect of nethike embrane is caused to be deteriorated, when selecting 150 ~ 400 object metal nethike embrane, nethike embrane is when super hydrophilic oleophobic state, can allow penetration by water nethike embrane and retain oil droplet ideally, nethike embrane is when super-hydrophobic oleophylic state, nethike embrane can utilize the hydrophobic oleophilic oil on surface, allow oil droplet penetrate and be unlikely to allow because of the pressure of water water through.
Further, in C step of the present invention, the concentration of long-chain alkanoic acid used or chain alkyl mercaptan ethanolic solution is 0.005 ~ 0.1mol/L.
Above-mentioned reaction is the alkyl structure in order to introduce long-chain on retinal surface micro-nano structure, alkyl structure is typical hydrophobic grouping, the hydrophilic and hydrophobic with control surface can be changed, when the concentration of long-chain alkanoic acid or chain alkyl mercaptan ethanolic solution is lower, enough long chain alkyl group can not be introduced in the surface of micro-nano structure, and alkyl group introducing reaction speed is slow, retinal surface does not reach super-hydrophobic effect or hydrophobic effect changes not obvious, when the concentration of long-chain alkanoic acid used or chain alkyl mercaptan ethanolic solution is higher, reaction speed is wayward, and the pattern of the micro-nano structure of retinal surface is damaged, therefore, the concentration that result of the test shows long-chain alkanoic acid used or chain alkyl mercaptan ethanolic solution controllably can change the hydrophilic and hydrophobic of retinal surface when being 0.005 ~ 0.1mol/L, and the structural intergrity of nethike embrane surface micro-nano structure can be protected preferably.
Further, in C step of the present invention, long-chain alkanoic acid used comprises dodecylic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, and chain alkyl mercaptan comprises lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
Above-mentioned reaction is the alkyl structure in order to introduce long-chain on retinal surface micro-nano structure, alkyl structure is typical hydrophobic grouping, the hydrophilic and hydrophobic with control surface can be changed, and the hydrophobicity of alkyl is relevant to the carbon chain lengths of alkyl, carbochain is longer, hydrophobicity is stronger, when carbon chain lengths is shorter, the hydrophobicity of retinal surface changes not obvious or hydrophobic effect is bad, when carbon chain lengths is larger, the hydrophobicity of nethike embrane can be significantly improved, when cost increases, therefore, consider from experiment effect and economic angle, in this patent, preferred long-chain alkanoic acid comprises dodecylic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, chain alkyl mercaptan comprises lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
Second goal of the invention of the present invention is to provide a kind of surface wettability method of converting of above-mentioned oil-water separation mesh film.The method can control separate mesh film surface wettability mutual fast transition between super hydrophilic oleophobic and super-hydrophobic oleophylic, and processing method is simple, and consuming time short, cost is low.
The present invention realizes the technical scheme that its second goal of the invention takes: a kind of surface wettability method of converting of above-mentioned oil-water separation mesh film, and its concrete operations are:
Immerse in the ethanolic solution of long-chain alkanoic acid or chain alkyl mercaptan to super hydrophilic-hydrophobic nethike embrane prepared by above-mentioned steps B, take out after soaking 1 ~ 30min under room temperature, with after alcohol flushing 1 ~ 3 time in 50 ~ 70 DEG C of oven drying 8 ~ 20min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by above-mentioned steps C, the time of thermal oxidation is 3 ~ 20min, and the temperature of thermal oxidation is 180 ~ 300 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
The principle of this technical scheme is:
Carry out simple wet-chemical treatment to super hydrophilic oleophobic nethike embrane prepared by step B, immersed by nethike embrane in the ethanolic solution of long-chain alkanoic acid or chain alkyl mercaptan, reaction certain hour, for metallic copper, reaction equation is:
Long-chain alkanoic acid: 2CH
3(CH
2)
ncOOH+CuO → Cu [CH
3(CH
2)
ncOO]
2+ H
2o
Long chain mercaptans: 2CH
3(CH
2)
nsH+CuO → Cu [CH
3(CH
2)
ns]
2+ H
2o
In reaction, the alkanoic acid of long-chain and the effect of alkyl hydrosulfide form one deck chain alkyl on the coarse web structure surface of above-mentioned preparation, thus the surface energy of degradation retinal surface micro-nano structure, promote that nethike embrane is to super-hydrophobic oleophylic state transfer.
In air atmosphere, thermal oxidation is carried out to the nethike embrane of the super-hydrophobic super-oleophylic obtained in step C, makes the chain alkyl molecular layer Oxidative demage of retinal surface, thus make nethike embrane change super hydrophilic super oleophobic into from super-hydrophobic oleophylic.For copper, the chemical equation of thermal oxidation is as follows:
Long-chain alkanoic acid: Cu [CH
3(CH
2)
ncOO]
2+ (3n+4) O
2→ CuO+ [2 (n+1)+1] H
2o+2 (n+2) CO
2
Long chain mercaptans: Cu [CH
3(CH
2)
ns]
2+ (3n+6) O
2→ CuO+ [2 (n+1)+1] H
2o+2 (n+2) SO
2+ 2 (n+2) CO
2
Compared with prior art, the beneficial effect of the technical program is:
Control to be separated nethike embrane surface wettability mutual fast transition between super hydrophilic oleophobic and super-hydrophobic oleophylic by simple thermal oxidation and wet chemistry method process, processing method is simple, and consuming time short, experiment parameter is controlled, and cost is low; Can according to the density of oil in oil water mixture, viscosity, the features such as mixed proportion, control targetedly be separated the wellability of nethike embrane or change the wellability of nethike embrane fast, thus realize being separated fast and efficiently oil water mixture.
Further, of the present inventionly change in the operation of super-hydrophobic oleophylic by the wellability of retinal surface by super hydrophilic oleophobic, the concentration of long-chain alkanoic acid used or chain alkyl mercaptan ethanolic solution is 0.005 ~ 0.1mol/L.
Further, of the present invention the wellability of retinal surface is changed in the operation of super-hydrophobic oleophylic by super hydrophilic oleophobic, long-chain alkanoic acid used comprises dodecylic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, chain alkyl mercaptan comprises lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
Accompanying drawing explanation
Fig. 1 is the SEM figure with the metal nethike embrane of micro-nano needle-like or ball bumps prepared by the embodiment of the present invention one steps A oxidizing process.
Fig. 2 is the super hydrophilic oleophobic oil-water separation mesh film prepared of the embodiment of the present invention one step B to the contact angle picture of diesel oil and water.
Fig. 3 is the super-hydrophobic oleophylic oil-water separation mesh film prepared of the embodiment of the present invention one step C to the contact angle picture of diesel oil and water.
Fig. 4 is the contact angle result of the embodiment of the present invention two oil-water separation mesh film wellability water and diesel oil when transforming between super hydrophilic oleophobic and super-hydrophobic oleophylic.
Detailed description of the invention
Embodiment one
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 0.5mol/L the alkaline medium of sodium hydroxide solution in, two potassium sulfates being 0.01mol/L by concentration are oxidized 150 object copper at its surface construction micro-nano structure, obtain the nethike embrane with other needle-like of micro-nano or ball bumps, the web structure with micro-nano needle-like or ball bumps of preparation as shown in Figure 1;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the copper mesh of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 3min, and the temperature of thermal oxidation is 300 DEG C; Taken out by nethike embrane after heat treatment, namely obtain super hydrophilic oleophobic nethike embrane, it to the contact angle experiments result of water and diesel oil as shown in Figure 2;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the dodecylic acid ethanolic solution of 0.005mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 1min under room temperature, with after alcohol flushing 1 time in 60 DEG C of oven drying 10min, namely obtain super-hydrophobic oleophylic nethike embrane, it to the contact angle experiments result of water and diesel oil as shown in Figure 3.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the dodecylic acid ethanolic solution of 0.005mol/L, take out after soaking 1min under room temperature, with after alcohol flushing 1 time in 60 DEG C of oven drying 10min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 3min, and the temperature of thermal oxidation is 300 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment two
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 7.5mol/L the alkaline medium of potassium hydroxide solution in, two metabisulfite solutions being 0.5mol/L by concentration are oxidized 200 object copper at its surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the copper mesh of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 3min, and the temperature of thermal oxidation is 300 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in tetradecanoic acid (myristic acid) ethanolic solution of 0.05mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 5min under room temperature, with after alcohol flushing 3 times in 60 DEG C of oven drying 10min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
D, the super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B are in the tetradecanoic acid ethanolic solution of 0.05mol/L, take out after soaking 5min under room temperature, with after alcohol flushing 3 times in 60 DEG C of oven drying 10min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
E, be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 3min, and the temperature of thermal oxidation is 300 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane;
By above-mentioned step D and step e, the wellability of fiber web material is transformed between super hydrophilic oleophobic and super-hydrophobic oleophylic state; Repeat above-mentioned D, E step 8 time respectively, test the contact angle to water and n-hexane of nethike embrane under each step, nethike embrane shows good structural stability, and its experimental result as shown in Figure 4.
Embodiment three
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 3mol/L the alkaline medium of sodium hydroxide solution in, two ammonium sulfates being 0.3mol/L by concentration are oxidized 400 object stainless (steel) wires at its surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the stainless (steel) wire of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 20min, and the temperature of thermal oxidation is 180 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the hexadecanoic acid ethanolic solution of 0.1mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 30min under room temperature, with after alcohol flushing 2 times in 50 DEG C of oven drying 8min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the hexadecanoic acid ethanolic solution of 0.1mol/L, take out after soaking 30min under room temperature, with after alcohol flushing 2 times in 50 DEG C of oven drying 8min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 20min, and the temperature of thermal oxidation is 180 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment four
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 1mol/L the alkaline medium of sodium hydroxide solution in, be that two ammonium sulfate of 0.3mol/L and two sodium sulphate mixed solutions are oxidized 400 object titanium nets at its surface construction micro-nano structure by concentration;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the titanium net of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the octadecanoid acid ethanolic solution of 0.005mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 20min under room temperature, with after alcohol flushing 2 times in 70 DEG C of oven drying 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the lauryl mercaptan ethanolic solution of 0.005mol/L, take out after soaking 25min under room temperature, with after alcohol flushing 2 times in 70 DEG C of oven drying 20min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment five
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 1mol/L the alkaline medium of sodium hydroxide solution in, two metabisulfite solutions being 0.3mol/L by concentration are oxidized 300 object aluminium nets at its surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the aluminium net of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the lauryl mercaptan ethanolic solution of 0.01mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 20min under room temperature, with after alcohol flushing 2 times in 70 DEG C of oven drying 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the octadecanoid acid ethanolic solution of 0.01mol/L, take out after soaking 15min under room temperature, with after alcohol flushing 2 times in 60 DEG C of oven drying 15min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment six
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 1mol/L the alkaline medium of sodium hydroxide solution in, two metabisulfite solutions being 0.3mol/L by concentration are oxidized 300 object aluminium nets at its surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the aluminium net of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the tetradecyl mercaptan ethanolic solution of 0.01mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 20min under room temperature, with after alcohol flushing 2 times in 70 DEG C of oven drying 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the Stearyl mercaptan ethanolic solution of 0.01mol/L, take out after soaking 15min under room temperature, with after alcohol flushing 2 times in 60 DEG C of oven drying 15min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment seven
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 1mol/L the alkaline medium of sodium hydroxide solution in, two metabisulfite solutions being 0.3mol/L by concentration are oxidized 300 object aluminium nets at its surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the aluminium net of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the hexadecyl mercaptan ethanolic solution of 0.01mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 20min under room temperature, with after alcohol flushing 2 times in 70 DEG C of oven drying 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the hexadecyl mercaptan ethanolic solution of 0.01mol/L, take out after soaking 15min under room temperature, with after alcohol flushing 2 times in 60 DEG C of oven drying 15min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment eight
A preparation method for oil-water separation mesh film, comprises the following steps:
A, in concentration be 1mol/L the alkaline medium of sodium hydroxide solution in, two metabisulfite solutions being 0.3mol/L by concentration are oxidized 300 object aluminium nets at its surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the aluminium net of micro-nano structure is placed in electric furnace, thermal oxidation in air atmosphere by the surface of preparing in steps A, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: it is in the Stearyl mercaptan ethanolic solution of 0.01mol/L that the super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration, take out after soaking 20min under room temperature, with after alcohol flushing 2 times in 70 DEG C of oven drying 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, its concrete operations are:
The super hydrophilic-hydrophobic nethike embrane immersion concentration prepared described step B is in the tetradecyl mercaptan ethanolic solution of 0.01mol/L, take out after soaking 15min under room temperature, with after alcohol flushing 2 times in 60 DEG C of oven drying 15min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Claims (10)
1. the preparation method of oil-water separation mesh film, comprises the following steps:
A, oxidizing process are at metal nethike embrane surface construction micro-nano structure;
B, thermal oxidation prepare super hydrophilic oleophobic nethike embrane: be that the metal nethike embrane of micro-nano structure is placed in electric furnace by the surface of preparing in steps A, thermal oxidation in air atmosphere, the time of thermal oxidation is 3 ~ 20min, and the temperature of thermal oxidation is 180 ~ 300 DEG C; Nethike embrane after heat treatment is taken out, namely obtains super hydrophilic oleophobic nethike embrane;
Super-hydrophobic oleophylic nethike embrane is prepared in C, wet chemistry method process: the super hydrophilic oleophobic nethike embrane prepared by step B immerses in the ethanolic solution of long-chain alkanoic acid or chain alkyl mercaptan, take out after soaking 1 ~ 30min under room temperature, with after alcohol flushing 1 ~ 3 time in 50 ~ 70 DEG C of oven drying 8 ~ 20min, namely obtain super-hydrophobic oleophylic nethike embrane.
2. the preparation method of oil-water separation mesh film according to claim 1, is characterized in that: in described A step, oxidizing process for construct micro-nano structure by dithionate oxidized metal nethike embrane in alkaline medium.
3. the preparation method of oil-water separation mesh film according to claim 2, is characterized in that: sodium hydroxide solution or the potassium hydroxide solution of described alkaline medium to be concentration be 0.5 ~ 7.5mol/L.
4. the preparation method of oil-water separation mesh film according to claim 2, is characterized in that: two potassium sulfate solutions of described dithionate to be concentration be 0.01 ~ 0.5mol/L, one or more mixed solution of two metabisulfite solutions or two ammonium sulfates.
5. the preparation method of oil-water separation mesh film according to claim 1, is characterized in that: described metal nethike embrane is 150 ~ 400 object copper mesh, stainless (steel) wire, titanium net or aluminium net.
6. the preparation method of oil-water separation mesh film according to claim 1, is characterized in that: in described C step, the concentration of long-chain alkanoic acid used or chain alkyl mercaptan ethanolic solution is 0.005 ~ 0.1mol/L.
7. the preparation method of the oil-water separation mesh film according to claim 1 or 6, it is characterized in that: in described C step, long-chain alkanoic acid used comprises dodecylic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, chain alkyl mercaptan comprises lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
8. a surface wettability method of converting for oil-water separation mesh film according to claim 1, its concrete operations are:
Immerse in the ethanolic solution of long-chain alkanoic acid or chain alkyl mercaptan to super hydrophilic-hydrophobic nethike embrane prepared by described step B, take out after soaking 1 ~ 30min under room temperature, with after alcohol flushing 1 ~ 3 time in 50 ~ 70 DEG C of oven drying 8 ~ 20min, namely the wellability of retinal surface changes super-hydrophobic oleophylic into by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane;
Be placed in electric furnace, thermal oxidation in air atmosphere to super-hydrophobic oleophylic nethike embrane prepared by described step C, the time of thermal oxidation is 3 ~ 20min, and the temperature of thermal oxidation is 180 ~ 300 DEG C; Taken out by nethike embrane after heat treatment, namely the wellability of nethike embrane changes super hydrophilic oleophobic into by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
9. the surface wettability method of converting of oil-water separation mesh film according to claim 8, it is characterized in that: describedly change in the operation of super-hydrophobic oleophylic by the wellability of retinal surface by super hydrophilic oleophobic, the concentration of long-chain alkanoic acid used or chain alkyl mercaptan ethanolic solution is 0.005 ~ 0.1mol/L.
10. the surface wettability method of converting of oil-water separation mesh film according to claim 8 or claim 9, it is characterized in that: described the wellability of retinal surface is changed in the operation of super-hydrophobic oleophylic by super hydrophilic oleophobic, long-chain alkanoic acid used comprises dodecylic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, chain alkyl mercaptan comprises lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
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