CN105268326B - The preparation of oil-water separation mesh film and its surface wettability method of converting - Google Patents
The preparation of oil-water separation mesh film and its surface wettability method of converting Download PDFInfo
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- CN105268326B CN105268326B CN201510642408.3A CN201510642408A CN105268326B CN 105268326 B CN105268326 B CN 105268326B CN 201510642408 A CN201510642408 A CN 201510642408A CN 105268326 B CN105268326 B CN 105268326B
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Abstract
A kind of preparation of oil-water separation mesh film and its surface wettability method of converting, separate the preparation step of nethike embrane: A, oxidizing process constructs micro-nano structure in metal retinal surface；B, the metal nethike embrane that the surface prepared in step A is micro-nano structure is placed in electric furnace, 3~20min of thermal oxidation in air atmosphere, the temperature of thermal oxidation is 180~300 DEG C；It takes out and obtains super hydrophilic oleophobic nethike embrane；C, the super hydrophilic oleophobic nethike embrane for preparing step B immerses in the ethanol solution of long alkanoic acid or chain alkyl mercaptan, at room temperature impregnate 1~30min after take out, after being rinsed with ethyl alcohol in 50~70 DEG C of 8~20min of oven drying to get arrive super-hydrophobic oleophylic nethike embrane.The processing of B step is carried out to super-hydrophobic oleophylic nethike embrane, step C processing is carried out to super hydrophilic oleophobic nethike embrane, i.e., changeable retinal surface wellability.This method is easy to operate, and the fiber web material separative efficiency of preparation is good, and can change its surface wettability by simple operations.
Description
Technical field
The invention belongs to the preparation fields of the semi-permeable membrane for separating technology, and in particular to a kind of surface wettability can change
Oil-water separation mesh film preparation and its surface wettability method of converting.
Background technique
It is many convenient and comfortable that expanding economy and the quickening of modernization are brought to human lives, while also bringing
The problems such as energy shortage and environmental pollution for becoming increasingly conspicuous.Such as oily pollution water, discharge of crude oil leakage and oily waste water etc. is to ring
Cause serious harm in border.Currently, oily water separation technique is obtained in multiple fields such as petrochemical industry, sewage treatment, food engineerings
To extensive use.But the difference of the factors such as organism kinds contained in oil mixing with water state, grease content and oil-water mixture,
Increase the difficulty of water-oil separating.Currently, oily water separation technique mainly has: the de- partition method of gravitational separation process, electricity, centrifuge separation
Method, method of chemical treatment and coarse separation method.But efficiency is lower, energy consumption is larger and chemical reagent caused by the limit such as secondary pollution
The application of above-mentioned facture is made.Therefore, the water-oil separating to oil water mixture and reusable how is effectively realized
Have become problem urgently to be resolved.
Since the surface tension between water and oil is there are larger difference, the selection oil material different with water logging lubricant nature can be with
The selective oil in oil water mixture is mutually and water phase carries out absorption and excretion, realizes to oily and water in oil water mixture
Separation.By the collective effect of surface microstructure and chemical composition, the available surface with special wellability, special leaching
The preparation on lubricant nature surface be mainly concerned with surface micro-nano roughness construct and surface chemical modification.The infiltration on reinforcing material surface
Property can effectively improve the efficiency of material water-oil separating.
Controllable immersing based on material surface, many super-hydrophobic oleophylic class separation fiber web materials are prepared out and are used for
Water-oil separating.But due to the difference of water and oil density, oil in the viscosity differences of different oils, and different oil water mixtures
The factors such as water ratio is uncertain, leading to above-mentioned separation material, there are still following disadvantages: first is that the oils small for density ratio water, oil
It bubbles through the water column, water, which tends to be formed between oil and super-hydrophobic oleophylic separation material superficial layer, to be stopped, to reduce the infiltration of oils
Thoroughly.Second is that the oils bigger for viscosity, can be adhered to net when through the web structure of super-hydrophobic oleophylic class separation material
Membrane material surface destroys material surface structure and reduces the wellability of material surface, to reduce its separative efficiency, and shortens and divides
The service life of off-network film.Third is that oil water mixture higher for oil content ratio, super-hydrophobic oleophylic class separation material selection
Separation oils greatly reduces the separative efficiency of material.
Summary of the invention
First invention purpose of the invention is to provide a kind of preparation method of oil-water separation mesh film.This method can prepare super parent
Water oleophobic nethike embrane and super-hydrophobic oleophylic nethike embrane, preparation process is simple, time-consuming short, oil-water separating net membrane material at low cost, and preparing
Expect that separative efficiency is good, there is good chemical stability and mechanical stability, long service life.
The present invention realizes that its first invention purpose is adopted the technical scheme that: a kind of preparation side of oil-water separation mesh film
Method, comprising the following steps:
A, oxidizing process constructs micro-nano structure in metal retinal surface；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: being the metal mesh of micro-nano structure by the surface prepared in step A
Film is placed in electric furnace, the thermal oxidation in air atmosphere, and the time of thermal oxidation is 3~20min, the temperature of thermal oxidation
Degree is 180~300 DEG C；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses long-chain
In the ethanol solution of alkanoic acid or chain alkyl mercaptan, at room temperature impregnate 1~30min after take out, with ethyl alcohol rinse 1~3 time after in
50~70 DEG C of 8~20min of oven drying to get arrive super-hydrophobic oleophylic nethike embrane.
The principle of the technical solution is:
Step A constructs micro-nano structure in metal retinal surface by oxidizing process, and step B passes through thermal oxidation for metal mesh
The metal of film surface is oxidized to metal oxide.The metal oxide nano coarse structure table with higher of metal retinal surface
Face energy, the surface water electrode Yi Qi infiltration, is presented hydrophilic and oleophobic characteristic；Under the state, water can be by nethike embrane, and oils cannot
By cover net film, to realize the water-oil separating of oil water mixture.
Step C carries out simple wet-chemical treatment to the super hydrophilic oleophobic nethike embrane of above-mentioned preparation, by the nethike embrane of above-mentioned preparation
It immerses in the ethanol solution of long alkanoic acid or chain alkyl mercaptan, reacts certain time, by taking metallic copper as an example, reaction equation
It is:
Long alkanoic acid: 2CH3(CH2)nCOOH+CuO→Cu[CH3(CH2)nCOO]2+H2O
Long chain mercaptans: 2CH3(CH2)nSH+CuO→Cu[CH3(CH2)nS]2+H2O
In reaction, the effect of the alkanoic acid and alkyl hydrosulfide of long-chain is to form one on the coarse web structure surface of above-mentioned preparation
Layer chain alkyl, so that the surface energy for the retinal surface micro-nano structure that degrades, promotes nethike embrane to change to super-hydrophobic oleophylic state.
Compared with prior art, the beneficial effect of the technical program is:
One, this method can prepare super hydrophilic oleophobic nethike embrane by simple thermal oxidation and wet chemistry method processing and surpass
Hydrophobic oleophilic oil nethike embrane, preparation process is simple, time-consuming short, at low cost, and the oil-water separating net membrane material separative efficiency prepared is good, tool
There are good chemical stability and mechanical stability, long service life.
Two, the oil-water separation mesh film surface wettability prepared can fast transition and controllable, can be according in oil water mixture
The density of oil, viscosity, the features such as mixed proportion, the targetedly wellability of control separation nethike embrane or the quickly leaching of change nethike embrane
Lubricant nature fast and efficiently separates oil water mixture to realize.
Further, oxidizing process is to pass through dithionate oxidized metal nethike embrane structure in alkaline medium in A step of the present invention
Build micro-nano structure.
Further, alkaline medium of the present invention is the sodium hydroxide solution or hydrogen-oxygen that concentration is 0.5~7.5mol/L
Change potassium solution.
Further, dithionate of the present invention is two potassium sulfate solutions that concentration is 0.01~0.5mol/L, two sulphur
One or more kinds of mixed solutions of acid sodium solution or two ammonium sulfates.
It is simple that micro-nano structure reaction condition is constructed by above-mentioned oxidizing process, can be carried out at room temperature, and micro-nano structure
It is fast to construct speed, time-consuming short, the micro-nano structure constructed is evenly distributed in retinal surface, ensure that the uniform of fiber web material performance
Property, and micro-nano structure has preferable chemical stability and structural stability, utilizes the service life for improving nethike embrane.
Further, metal nethike embrane of the present invention is the copper mesh of 150~400 mesh, stainless (steel) wire, titanium net or aluminium net.
In oil water mixture, oil is that a few micrometers of droplet-likes to hundreds of microns are distributed in water with diameter, and nethike embrane mesh number is got over
Greatly, retinal surface aperture is smaller, improves to the separating effect of oil water mixture, but water is increased by the difficulty in aperture, nethike embrane
Separative efficiency reduces, and nethike embrane mesh number is smaller, and retinal surface aperture is bigger, and the oil droplet in oil water mixture penetrates readily through nethike embrane,
The separating effect of nethike embrane is caused to be deteriorated, when selecting the metal nethike embrane of 150~400 mesh, nethike embrane is in super hydrophilic oleophobic state, energy
It reaches and ideally allows penetration by water nethike embrane and retain oil droplet, for nethike embrane in super-hydrophobic oleophylic state, nethike embrane can utilize the hydrophobic of surface
Lipophilicity allows oil droplet to penetrate and is unlikely to allow water to penetrate because of the pressure of water.
Further, the concentration of long alkanoic acid used in C step of the present invention or chain alkyl mercaptan ethanol 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, and alkyl structure is typical
The hydrophilic and hydrophobic on surface can be varied and controlled in hydrophobic grouping, when the concentration of long alkanoic acid or chain alkyl mercaptan ethanol solution
When lower, the surface of micro-nano structure cannot introduce enough long chain alkyl groups, and alkyl group introducing reaction speed is slow, nethike embrane
Super-hydrophobic effect is not achieved in surface or hydrophobic effect change is unobvious, when long alkanoic acid or chain alkyl mercaptan ethyl alcohol used is molten
When the concentration of liquid is higher, reaction speed is not easy to control, and the pattern of the micro-nano structure of retinal surface is destroyed, therefore, test
It can be controllable when the concentration of long alkanoic acid used or chain alkyl mercaptan ethanol solution is 0.005~0.1mol/L as the result is shown
Ground changes the hydrophilic and hydrophobic of retinal surface, and can preferably protect the structural intergrity of retinal surface micro-nano structure.
Further, long alkanoic acid used in C of the present invention step includes dodecanoic acid, tetradecanoic acid, hexadecanoic acid or
Octadecanoid acid, chain alkyl mercaptan include lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or octadecyl sulphur
Alcohol.
Above-mentioned reaction is the alkyl structure in order to introduce long-chain on retinal surface micro-nano structure, and alkyl structure is typical
The hydrophilic and hydrophobic on surface can be varied and controlled in hydrophobic grouping, and the hydrophobicity of alkyl is related to the carbon chain lengths of alkyl, carbochain
Longer, hydrophobicity is stronger, and when carbon chain lengths are shorter, to sexually revise unobvious or hydrophobic effect bad for retinal surface hydrophobic, when
When carbon chain lengths are larger, the hydrophobicity of nethike embrane can be significantly improved, works as increased costs, therefore, from experiment effect and economic angle
Consider, preferred long alkanoic acid includes dodecanoic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, chain alkyl in this patent
Mercaptan includes lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
Second goal of the invention of the invention is to provide a kind of surface wettability method of converting of above-mentioned oil-water separation mesh film.It should
Controllable separation retinal surface wellability mutual fast transition, the processing method between super hydrophilic oleophobic and super-hydrophobic oleophylic of method
Simply, time-consuming short, it is at low cost.
The present invention realizes that its second goal of the invention is adopted the technical scheme that: a kind of table of above-mentioned oil-water separation mesh film
Face wellability method of converting, concrete operations are as follows:
The ethanol solution of long alkanoic acid or chain alkyl mercaptan is immersed to the super hydrophilic hydrophobic nethike embrane of above-mentioned steps B preparation
In, it is taken out after impregnating 1~30min at room temperature, in 50~70 DEG C of 8~20min of oven drying, nethike embrane after being rinsed 1~3 time with ethyl alcohol
The wellability on surface is changed into super-hydrophobic oleophylic by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of above-mentioned steps C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 3~20min, and the temperature of thermal oxidation is 180~300 DEG C；Nethike embrane after heat treatment is taken out, nethike embrane
Wellability super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtain super hydrophilic oleophobic nethike embrane.
The principle of the technical solution is:
Simple wet-chemical treatment is carried out to the super hydrophilic oleophobic nethike embrane of step B preparation, by nethike embrane immerse long alkanoic acid or
In the ethanol solution of chain alkyl mercaptan, certain time is reacted, by taking metallic copper as an example, reaction equation is:
Long alkanoic acid: 2CH3(CH2)nCOOH+CuO→Cu[CH3(CH2)nCOO]2+H2O
Long chain mercaptans: 2CH3(CH2)nSH+CuO→Cu[CH3(CH2)nS]2+H2O
In reaction, the effect of the alkanoic acid and alkyl hydrosulfide of long-chain is to form one on the coarse web structure surface of above-mentioned preparation
Layer chain alkyl, so that the surface energy for the retinal surface micro-nano structure that degrades, promotes nethike embrane to change to super-hydrophobic oleophylic state.
Thermal oxidation is carried out in air atmosphere to the nethike embrane of the super-hydrophobic super-oleophylic obtained in step C, makes nethike embrane table
The chain alkyl molecular layer Oxidative demage in face, so that nethike embrane be made to be changed into superhydrophilic superoleophobic from super-hydrophobic oleophylic.By taking copper as an example,
The chemical equation of thermal oxidation is as follows:
Long alkanoic acid: Cu [CH3(CH2)nCOO]2+(3n+4)O2→CuO+[2(n+1)+1]H2O+2(n+2)CO2
Long chain mercaptans: Cu [CH3(CH2)nS]2+(3n+6)O2→CuO+[2(n+1)+1]H2O+2(n+2)SO2+2(n+2)CO2
Compared with prior art, the beneficial effect of the technical program is:
By simple thermal oxidation and wet chemistry method processing control separation retinal surface wellability in super hydrophilic oleophobic
The mutual fast transition between super-hydrophobic oleophylic, processing method is simple, and time-consuming short, experiment parameter is controllable, at low cost；It can basis
Oily density in oil water mixture, viscosity, the features such as mixed proportion, targetedly control separates the wellability or quick of nethike embrane
Change the wellability of nethike embrane, oil water mixture is fast and efficiently separated to realize.
Further, the wellability of the present invention by retinal surface is changed into the operation of super-hydrophobic oleophylic by super hydrophilic oleophobic
In, the concentration of long alkanoic acid used or chain alkyl mercaptan ethanol solution is 0.005~0.1mol/L.
Further, the wellability of the present invention by retinal surface is changed into the operation of super-hydrophobic oleophylic by super hydrophilic oleophobic
In, long alkanoic acid used includes dodecanoic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, and chain alkyl mercaptan includes ten
Dialkyl group mercaptan, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
Detailed description of the invention
Fig. 1 has micro-nano needle-shaped or the metal nethike embrane of ball bumps for the preparation of one step A oxidizing process of the embodiment of the present invention
SEM figure.
Fig. 2 is contact of the super hydrophilic oleophobic oil-water separation mesh film of one step B of embodiment of the present invention preparation to diesel oil with water
Angle picture.
Fig. 3 is contact of the super-hydrophobic oleophylic oil-water separation mesh film of one step C of embodiment of the present invention preparation to diesel oil with water
Angle picture.
Fig. 4 is that two oil-water separation mesh film wellability of the embodiment of the present invention converts between super hydrophilic oleophobic and super-hydrophobic oleophylic
The contact angle result of Shi Shui and diesel oil.
Specific embodiment
Embodiment one
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
It A, is the two of 0.01mol/L by concentration in the alkaline medium for the sodium hydroxide solution that concentration is 0.5mol/L
Potassium sulfate aoxidizes the copper of 150 mesh in its surface construction micro-nano structure, obtains having micro-nano other needle-shaped or ball bumps nets
Film, preparation with micro-nano is needle-shaped or the web structure of ball bumps is as shown in Figure 1；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the copper mesh that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 3min, and the temperature of thermal oxidation is 300
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived, to the contact angle experiments result such as figure of water and diesel oil
Shown in 2；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 1min at room temperature in the dodecanoic acid ethanol solution of 0.005mol/L, dried after being rinsed 1 time with ethyl alcohol in 60 DEG C
The dry 10min of case is as shown in Figure 3 to the contact angle experiments result of water and diesel oil to get arriving super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The dodecanoic acid ethanol solution that concentration is 0.005mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
In, it is taken out after impregnating 1min at room temperature, in 60 DEG C of oven drying 10min after being rinsed 1 time with ethyl alcohol, the wellability of retinal surface is
Super-hydrophobic oleophylic is changed by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 3min, and the temperature of thermal oxidation is 300 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment two
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the potassium hydroxide solution that concentration is 7.5mol/L, two sulphur for being 0.5mol/L by concentration
Acid sodium solution aoxidizes the copper of 200 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the copper mesh that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 3min, and the temperature of thermal oxidation is 300
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 5min at room temperature in tetradecanoic acid (myristic acid) ethanol solution of 0.05mol/L, rinsed 3 times with ethyl alcohol
Afterwards in 60 DEG C of oven drying 10min to get arrive super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
D, molten for the tetradecanoic acid ethyl alcohol of 0.05mol/L to the super hydrophilic hydrophobic nethike embrane immersion concentration of step B preparation
It in liquid, is taken out after impregnating 5min at room temperature, in 60 DEG C of oven drying 10min, the wellability of retinal surface after being rinsed 3 times with ethyl alcohol
Super-hydrophobic oleophylic is changed by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
E, the super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, heat
The time of oxidation processes is 3min, and the temperature of thermal oxidation is 300 DEG C；Nethike embrane after heat treatment is taken out, the infiltration of nethike embrane
Property super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtain super hydrophilic oleophobic nethike embrane；
D and step E makes the wellability of fiber web material in super hydrophilic oleophobic and super-hydrophobic oleophylic state through the above steps
Between convert；Above-mentioned D, E step 8 time is repeated respectively, tests contact angle of the nethike embrane to water and n-hexane, nethike embrane table under each step
Good structural stability is revealed, experimental result is as shown in Figure 4.
Embodiment three
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the sodium hydroxide solution that concentration is 3mol/L, two sulfuric acid for being 0.3mol/L by concentration
Ammonium salt solution aoxidizes the stainless (steel) wire of 400 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: being the stainless steel of micro-nano structure by the surface prepared in step A
Net is placed in electric furnace, the thermal oxidation in air atmosphere, and the time of thermal oxidation is 20min, the temperature of thermal oxidation
It is 180 DEG C；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 30min at room temperature in the hexadecanoic acid ethanol solution of 0.1mol/L, dried after being rinsed 2 times with ethyl alcohol in 50 DEG C
Case dries 8min to get super-hydrophobic oleophylic nethike embrane is arrived.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The hexadecanoic acid ethanol solution that concentration is 0.1mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
In, it is taken out after impregnating 30min at room temperature, in 50 DEG C of oven drying 8min after being rinsed 2 times with ethyl alcohol, the wellability of retinal surface is
Super-hydrophobic oleophylic is changed by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 20min, and the temperature of thermal oxidation is 180 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Example IV
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the sodium hydroxide solution that concentration is 1mol/L, two sulfuric acid for being 0.3mol/L by concentration
Ammonium and two sodium sulphate mixed solutions aoxidize the titanium net of 400 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the titanium net that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 20min at room temperature in the octadecanoid acid ethanol solution of 0.005mol/L, in 70 DEG C after being rinsed 2 times with ethyl alcohol
Oven drying 20min to get arrive super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The lauryl mercaptan ethyl alcohol that concentration is 0.005mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
It in solution, is taken out after impregnating 25min at room temperature, in 70 DEG C of oven drying 20min, the leaching of retinal surface after being rinsed 2 times with ethyl alcohol
Lubricant nature is changed into super-hydrophobic oleophylic by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 10min, and the temperature of thermal oxidation is 250 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment five
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the sodium hydroxide solution that concentration is 1mol/L, two sulfuric acid for being 0.3mol/L by concentration
Sodium solution aoxidizes the aluminium net of 300 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the aluminium net that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 20min at room temperature in the lauryl mercaptan ethanol solution of 0.01mol/L, in 70 after being rinsed 2 times with ethyl alcohol
DEG C oven drying 20min is to get arriving super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The octadecanoid acid ethanol solution that concentration is 0.01mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
In, it is taken out after impregnating 15min at room temperature, in 60 DEG C of oven drying 15min, the wellability of retinal surface after being rinsed 2 times with ethyl alcohol
Super-hydrophobic oleophylic is changed by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 10min, and the temperature of thermal oxidation is 250 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment six
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the sodium hydroxide solution that concentration is 1mol/L, two sulfuric acid for being 0.3mol/L by concentration
Sodium solution aoxidizes the aluminium net of 300 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the aluminium net that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 20min at room temperature in the tetradecyl mercaptan ethanol solution of 0.01mol/L, in 70 after being rinsed 2 times with ethyl alcohol
DEG C oven drying 20min is to get arriving super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The Stearyl mercaptan ethyl alcohol that concentration is 0.01mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
It in solution, is taken out after impregnating 15min at room temperature, in 60 DEG C of oven drying 15min, the leaching of retinal surface after being rinsed 2 times with ethyl alcohol
Lubricant nature is changed into super-hydrophobic oleophylic by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 10min, and the temperature of thermal oxidation is 250 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment seven
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the sodium hydroxide solution that concentration is 1mol/L, two sulfuric acid for being 0.3mol/L by concentration
Sodium solution aoxidizes the aluminium net of 300 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the aluminium net that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 20min at room temperature in the hexadecyl mercaptan ethanol solution of 0.01mol/L, in 70 after being rinsed 2 times with ethyl alcohol
DEG C oven drying 20min is to get arriving super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The hexadecyl mercaptan ethyl alcohol that concentration is 0.01mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
It in solution, is taken out after impregnating 15min at room temperature, in 60 DEG C of oven drying 15min, the leaching of retinal surface after being rinsed 2 times with ethyl alcohol
Lubricant nature is changed into super-hydrophobic oleophylic by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 10min, and the temperature of thermal oxidation is 250 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Embodiment eight
A kind of preparation method of oil-water separation mesh film, comprising the following steps:
A, in the alkaline medium for the sodium hydroxide solution that concentration is 1mol/L, two sulfuric acid for being 0.3mol/L by concentration
Sodium solution aoxidizes the aluminium net of 300 mesh in its surface construction micro-nano structure；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the aluminium net that the surface prepared in step A is micro-nano structure is set
In electric furnace, the thermal oxidation in air atmosphere, the time of thermal oxidation is 10min, and the temperature of thermal oxidation is 250
℃；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses concentration
To be taken out after impregnating 20min at room temperature in the Stearyl mercaptan ethanol solution of 0.01mol/L, in 70 after being rinsed 2 times with ethyl alcohol
DEG C oven drying 20min is to get arriving super-hydrophobic oleophylic nethike embrane.
The surface wettability method of converting of above-mentioned oil-water separation mesh film, concrete operations are as follows:
The tetradecyl mercaptan ethyl alcohol that concentration is 0.01mol/L is immersed to the super hydrophilic hydrophobic nethike embrane of step B preparation
It in solution, is taken out after impregnating 15min at room temperature, in 60 DEG C of oven drying 15min, the leaching of retinal surface after being rinsed 2 times with ethyl alcohol
Lubricant nature is changed into super-hydrophobic oleophylic by super hydrophilic oleophobic, obtains super-hydrophobic oleophylic nethike embrane；
The super-hydrophobic oleophylic nethike embrane of step C preparation is placed in electric furnace, the thermal oxidation in air atmosphere, hot oxygen
The time for changing processing is 10min, and the temperature of thermal oxidation is 250 DEG C；Nethike embrane after heat treatment is taken out, the wellability of nethike embrane
Super hydrophilic oleophobic is changed by super-hydrophobic oleophylic, obtains super hydrophilic oleophobic nethike embrane.
Claims (7)
1. the preparation method of oil-water separation mesh film, comprising the following steps:
A, oxidizing process constructs micro-nano structure in metal retinal surface；
The oxidizing process is to construct micro-nano structure by dithionate oxidized metal nethike embrane in alkaline medium；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the metal nethike embrane that the surface prepared in step A is micro-nano structure is set
In electric furnace, the time of the thermal oxidation in air atmosphere, thermal oxidation is 3~20min, and the temperature of thermal oxidation is
180~300 DEG C；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived.
2. the preparation method of oil-water separation mesh film, comprising the following steps:
A, oxidizing process constructs micro-nano structure in metal retinal surface；
The oxidizing process is to construct micro-nano structure by dithionate oxidized metal nethike embrane in alkaline medium；
B, thermal oxidation prepares super hydrophilic oleophobic nethike embrane: the metal nethike embrane that the surface prepared in step A is micro-nano structure is set
In electric furnace, the time of the thermal oxidation in air atmosphere, thermal oxidation is 3~20min, and the temperature of thermal oxidation is
180~300 DEG C；Nethike embrane after heat treatment is taken out to get super hydrophilic oleophobic nethike embrane is arrived；
C, wet chemistry method processing prepares super-hydrophobic oleophylic nethike embrane: super hydrophilic oleophobic nethike embrane prepared by step B immerses long alkanoic acid
Or in the ethanol solution of chain alkyl mercaptan, taken out after impregnating 1~30min at room temperature, after being rinsed 1~3 time with ethyl alcohol in 50~
70 DEG C of 8~20min of oven drying to get arrive super-hydrophobic oleophylic nethike embrane.
3. the preparation method of oil-water separation mesh film according to claim 1 or 2, it is characterised in that: the alkaline medium is
Concentration is the sodium hydroxide solution or potassium hydroxide solution of 0.5~7.5mol/L.
4. the preparation method of oil-water separation mesh film according to claim 1 or 2, it is characterised in that: the dithionate is
Concentration is two potassium sulfate solutions of 0.01~0.5mol/L, the one or more of two metabisulfite solutions or two ammonium sulfates
Mixed solution.
5. the preparation method of oil-water separation mesh film according to claim 1 or 2, it is characterised in that: the metal nethike embrane is
The copper mesh of 150~400 mesh, stainless (steel) wire, titanium net or aluminium net.
6. the preparation method of oil-water separation mesh film according to claim 2, it is characterised in that: long used in the C step
The concentration of the ethanol solution of alkanoic acid or chain alkyl mercaptan is 0.005~0.1mol/L.
7. the preparation method of the oil-water separation mesh film according to claim 2 or 6, it is characterised in that: used in the C step
Long alkanoic acid includes dodecanoic acid, tetradecanoic acid, hexadecanoic acid or octadecanoid acid, and chain alkyl mercaptan includes dodecyl sulphur
Alcohol, tetradecyl mercaptan, hexadecyl mercaptan or Stearyl mercaptan.
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| CN117101186B (en) * | 2023-06-21 | 2024-04-02 | 中南民族大学 | Method for regulating and controlling wettability of oil-water separation material |
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