CN109351204A - A kind of preparation method and application of fluorine-containing aquagel membrane - Google Patents
A kind of preparation method and application of fluorine-containing aquagel membrane Download PDFInfo
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- CN109351204A CN109351204A CN201811063422.8A CN201811063422A CN109351204A CN 109351204 A CN109351204 A CN 109351204A CN 201811063422 A CN201811063422 A CN 201811063422A CN 109351204 A CN109351204 A CN 109351204A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- 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
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- 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
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
Abstract
The invention discloses a kind of preparation method and applications of fluorine-containing aquagel membrane, belong to water-oil separationg film preparation technical field.It include: after (1) will clean up in fabric immersion acetone, to dry at normal temperature；(2) acrylate containing fluorine monomer, hydrophilic monomer, crosslinking agent and reducing agent are dissolved in methanol and are stirred evenly, obtain mixed solution；(3) oxidant is dissolved in methanol；(4) mixed solution that step (2) obtains quickly is mixed with aqueous solution in step (3), is uniformly coated on the surface of the fabric after step (1) is dried；(5) so that monomer is carried out polymerisation in solution under the action of redox initiator, form organic gel layer in fabric surface；(6) it is immersed in distilled water, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.To sum up, method of the invention is easy to operate, is easy to large scale preparation, and manufactured fluorine-containing aquagel membrane intensity is high and at low cost, carries out the high-efficient of water-oil separating.
Description
Technical field
The present invention relates in water-oil separationg film preparation and applied technical field, be specifically to provide a kind of fluorine-containing aquagel membrane
Preparation method and application.
Background technique
In recent years, the continuous research comprehensive with each field, hydrogel as a kind of high score with multiple functions
The application demand of sub- polymeric material is more and more extensive, and the advantage of the exclusive hydrophily of hydrogel and biocompatibility has caused
The concern of materials science and biological medicine circle.And macromolecule hydrogel is a kind of polymer network knot for containing a large amount of water
Structure, in organizational project, also there are very important research significance and application prospect in water-oil separating water purification decontamination field.Water-setting simultaneously
The superpower water absorbency and water retentivity of glue more makes it be widely used in industrial super strength water absorbent and agricultural soil water-retaining agent, as a kind of fast
Fast adsorption and desorption, high-efficiency adsorbent that is easily separated and repeating to recycle have in terms of administering water pollution very big application and
Research.
In the prior art, patent CN102029079A is related to oil-water separation mesh film and its system with underwater superoleophobic property
Preparation Method and purposes.The oil-water separation mesh film of the invention is using 100~400 mesh fabric web as substrate, using light-initiated poly-
The method of conjunction obtains the hydrogel clad formed with polymer monomer cross-linked polymeric, to obtain on the twine of fabric web
The nethike embrane of the invention.The oil-water separation mesh film of the invention has in air and super hydrophilic under water and superoleophobic under water property
Matter is greater than 150 ° to the contact angle of oil droplet under water, and has the characteristic to the low adherency of oil droplet.The nethike embrane of the invention can be applied
In oily waste water treatment, Chemical Decomposition and environmental protection etc..Carrying out water-oil separating with the nethike embrane has good separating effect, divides
, low cost fast from speed, low energy consumption, conveniently, easily recycled without other chemical addition agents, nethike embrane and be used repeatedly, can be used for
A wide range of preparation can the advantages that.
Summary of the invention
To solve the problems of the prior art, the present invention provides a kind of preparation method and application of fluorine-containing aquagel membrane, this
The water-oil separationg film molding time for inventing the superhydrophilic superoleophobic property of preparation is short, can be used for oily wastewater and oil-in-water emulsion
Separation, separating rate is fast, high-efficient, and at low cost, and production equipment and production routine are simple, is easy to large scale preparation.
In order to solve the above technical problems, present invention offer technical solution is as follows:
On the one hand, the present invention provides a kind of preparation method of fluorine-containing aquagel membrane, after being the hydrophilic treated by 150-300 mesh
Fabric web as substrate, by Redox Initiator acrylate containing fluorine monomer and acrylamide or acrylic monomer into
Row polymerisation in solution obtains the hydrogel clad that polymerization is formed on the fabric, so that a kind of composite membrane is obtained, it is as of the invention
Fluorine-containing aquagel membrane；Include:
(1) fabric is immersed in acetone and is carried out ultrasound 30 minutes, after cleaning up, dried at normal temperature；
(2) at 5-40 DEG C, acrylate containing fluorine monomer, hydrophilic monomer, crosslinking agent and reducing agent are dissolved in methanol
In and stir evenly, lead to nitrogen remove mixed solution in oxygen, obtain mixed solution；
(3) oxidant is dissolved in methanol；
(4) mixed solution that step (2) obtains quickly is mixed with aqueous solution in step (3), is uniformly coated on step
(1) then the surface of the fabric after drying leads to nitrogen and removes oxygen；
(5) 10-30 minutes are stood at 5-40 DEG C, draws acrylate containing fluorine monomer and hydrophilic monomer in redox
Polymerisation in solution is carried out under the action of hair agent, forms organic gel layer in fabric surface；
(6) it is immersed in distilled water 12-96 hours, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.
Further, in the step (1), fabric is nylon, polyvinyl, aramid fiber, terylene or the acrylic fiber of 150-300 mesh
Fabric.
Further, in the step (2), acrylate containing fluorine monomer is trifluoroethyl methacrylate, methyl-prop
Olefin(e) acid tetrafluoro propyl ester, Hexafluorobutyl mathacrylate, methacrylic acid perfluoro butyl ethyl ester, ten difluoro heptan of methacrylic acid
One of ester, methacrylic acid perfluoro hexyl ethyl ester are a variety of.
Further, in the step (2), hydrophilic monomer be acrylamide, acrylic acid, sodium acrylate, potassium acrylate,
One of polyalkylene glycol acrylate is a variety of.
Further, in the step (2), crosslinking agent N, N '-methylene-bisacrylamide, polyethylene glycol dimethyl propylene
One of olefin(e) acid ester, ethylene glycol dimethacrylate are a variety of.
Further, in the step (2), reducing agent N, N- dimethyl-p-toluidine or n,N-Dimethylaniline.
Further, in the step (2), the content of acrylate containing fluorine monomer is 1-10wt%, parent in mixture
The content of aqueous monomers is 20-30wt%；The content of crosslinking agent is 0.2-0.8wt%, the content of oxidant is 0.4-
The content of 0.8wt%, reducing agent are 0.1-0.4wt%, and surplus is methanol.
Further, in the step (3), oxidant is benzoyl peroxide, cyclohexanone peroxide, methyl ethyl ketone peroxide
Or diphenyl peroxide first phthalein.
Further, the fluorine-containing aquagel membrane of preparation is lower than 40 ° to the contact angle of water droplet, is greater than to the contact angle of oil droplet
120 °, roll angle is lower than 25 °, and alcohol content is greater than 85%.
On the other hand, the present invention also provides a kind of fluorine-containing aquagel membranes of the preparation method preparation of above-mentioned fluorine-containing aquagel membrane
Application, the separation for oily wastewater and oil-in-water emulsion.
Compared with prior art, the invention has the following advantages:
The present invention provides a kind of preparation method and application of fluorine-containing aquagel membrane, successfully prepares with superhydrophilic superoleophobic
The water-oil separationg film of property, and water-oil separationg film molding time is short, can be used for the separation of oily wastewater and oil-in-water emulsion, separation
Speed is fast, high-efficient, and at low cost, and production equipment and production routine are simple, is easy to large scale preparation.Grease of the invention point
It is lower than 40 ° from contact angle of the film to water droplet, 120 ° is greater than to the contact angle of oil droplet, roll angle is lower than 25 °, and water-oil separating is high-efficient
Up to 99.69%.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, specific embodiment will be used below
It is described in detail, but the present invention is limited to absolutely not these examples.The following is only the preferred embodiment of the present invention, is only used to
Explain the present invention, it cannot be construed as a limitation to the scope of the present invention.It should be pointed out that all of the invention
Any modifications, equivalent replacements, and improvements etc. done within spirit and principle, should all be included in the protection scope of the present invention.
Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Except specified otherwise, component used in the present invention is commercial product.
The present invention provides a kind of preparation method and application of fluorine-containing aquagel membrane, and specific embodiment is as follows.
Embodiment 1
A kind of preparation method of fluorine-containing aquagel membrane, comprising:
(1) the nylon fabric net of 200 mesh is immersed in acetone and is cleaned by ultrasonic 30 minutes, dried under room temperature；
(2) at 10 DEG C, 11.66g methanol is added in 20ml serum bottle, by 0.2g trifluoroethyl methacrylate, 6g
Acrylamide, 0.04g N, N '-methylene-bisacrylamide and 0.02gN, N- dimethyl-p-toluidine are dissolved in methanol, magnetic force
It is uniformly mixed, leads to nitrogen half an hour, remove the oxygen in mixed solution, obtain mixed solution；
(3) 0.08g benzoyl peroxide is dissolved in 2g methanol again, is uniformly mixed；
(4) it after quickly mixing the mixed solution that step (2) obtains with methanol solution in step (3), is uniformly coated on
Step (1) dry after nylon wire surface, lead to nitrogen half an hour, remove oxygen；
(5) 10 DEG C of standing 10min, make trifluoroethyl methacrylate and acrylamide in the effect of redox initiator
Lower carry out polymerisation in solution forms organic gel layer in fabric surface；
(6) it is immersed in distilled water 12 hours, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.
Fluorine-containing aquagel membrane prepared by the above method detects its contact angle, the contact angle to water is 20 °, to just
The contact angle of hexane oil droplet is 110 °, and 20 ° of roll angle, aperture is 15-20 μm.
Use non-woven fabrics as support above-mentioned fluorine-containing aquagel membrane, it is real to carry out water-oil separating using Simple oil-water separator
It tests, by the mixture (volume ratio 3: 2, magnetic agitation 25 minutes, 20-30 μm of oil droplet size) of preprepared vegetable oil and water
It is poured on fluorine-containing aquagel membrane, under the pressure less than 0.02MPa, water passes through fluorine-containing aquagel membrane and flows out from below, simultaneously
Vegetable oil is blocked in above fluorine-containing aquagel membrane, and separative efficiency is up to 99.63%, realizes the mesh of oil-water separation mixture
's.
Embodiment 2
A kind of preparation method of fluorine-containing aquagel membrane, comprising:
(1) the aramid fabric net of 300 mesh is immersed in acetone and is cleaned by ultrasonic 30 minutes, dried under room temperature；
At (2) 25 DEG C, 15.2g methanol is added in 20ml serum bottle, by 1.25g tetrafluoropropyl propyl ester, 6.25g
Acrylic acid, 0.1g polyethylene glycol dimethacrylate and 0.05gN, accelerine are dissolved in methanol, magnetic agitation mixing
Uniformly, lead to nitrogen half an hour, remove the oxygen in mixed solution, obtain mixed solution；
(3) 0.15g cyclohexanone peroxide is dissolved in 2g methanol again, is uniformly mixed；
(4) it after quickly mixing the mixed solution that step (2) obtains with methanol solution in step (3), is uniformly coated on
Step (1) dry after aramid fabric net surface, lead to nitrogen half an hour, remove oxygen；
(5) 25 DEG C of standing 20min, make tetrafluoropropyl propyl ester and acrylic acid under the action of redox initiator
Polymerisation in solution is carried out, forms organic gel layer in fabric surface；
(6) it is immersed in distilled water 48 hours, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.
Fluorine-containing aquagel membrane prepared by the above method detects its contact angle, the contact angle to water is 30 °, to just
The contact angle of hexane oil droplet is 115 °, and 15 ° of roll angle, aperture is 10-20 μm.
It uses the steel wire of 100 mesh as support above-mentioned fluorine-containing aquagel membrane, carries out oil using Simple oil-water separator
Water separating experiment, by the mixture of preprepared n-hexane and water (volume ratio 4: 7, magnetic agitation 30 minutes, oil droplet size
30-35 μm) it is poured on fluorine-containing aquagel membrane, under the pressure less than 0.04MPa, water passes through fluorine-containing aquagel membrane and flows from below
Out, while n-hexane is blocked in the top of fluorine-containing aquagel membrane, and separative efficiency is up to 99.69%, and it is mixed to realize oil-water separation
Close the purpose of object.
Embodiment 3
A kind of preparation method of fluorine-containing aquagel membrane, comprising:
(1) the acrylic fiber fabric web of 150 mesh is immersed in acetone and is cleaned by ultrasonic 30 minutes, dried under room temperature；
(2) at 40 DEG C, 15.64g methanol is added in 25ml serum bottle, by 3g Hexafluorobutyl mathacrylate, 9g third
Olefin(e) acid polyethylene glycol (molecular weight 300), 0.24g ethylene glycol dimethacrylate and 0.12gN, N- dimethyl-p-toluidine are molten
In methanol, magnetic agitation is uniformly mixed, and leads to nitrogen half an hour, is removed the oxygen in mixed solution, is obtained mixed solution；
(3) 0.24g methyl ethyl ketone peroxide is dissolved in 2g methanol again, is uniformly mixed；
(4) it after quickly mixing the mixed solution that step (2) obtains with methanol solution in step (3), is uniformly coated on
Step (1) dry after acrylic fiber fabric web surface, lead to nitrogen half an hour, remove oxygen；
(5) 40 DEG C of standing 30min, make Hexafluorobutyl mathacrylate and polyalkylene glycol acrylate in redox initiator
Under the action of carry out polymerisation in solution, form organic gel layer in fabric surface；
(6) it is immersed in distilled water 96 hours, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.
Fluorine-containing aquagel membrane prepared by the above method detects its contact angle, the contact angle to water is 35 °, to just
The contact angle of hexane oil droplet is 120 °, and 10 ° of roll angle, aperture is 20-25 μm.
Use non-woven fabrics as support above-mentioned fluorine-containing aquagel membrane, it is real to carry out water-oil separating using Simple oil-water separator
It tests, by the mixture (volume ratio 1: 1, magnetic agitation 20 minutes, 30-40 microns of oil droplet size) of preprepared diesel oil and water
It is poured on fluorine-containing aquagel membrane, under the pressure less than 0.04MPa, water passes through fluorine-containing aquagel membrane and flows out from below, simultaneously
Diesel oil is blocked in the top of fluorine-containing aquagel membrane, and separative efficiency is up to 99.28%, realizes the mesh of oil-water separation mixture
's.
For the performance for further proving fluorine-containing aquagel membrane prepared by the present invention, because length is limited, only by taking embodiment 2 as an example
It is as follows to construct comparative example.
Comparative example 1
A kind of preparation method of fluorine-containing aquagel membrane, comprising:
(1) the aramid fabric net of 300 mesh is immersed in acetone and is cleaned by ultrasonic 30 minutes, dried under room temperature；
At (2) 25 DEG C, 17.2g methanol is added in 20ml serum bottle, by 1.25g tetrafluoropropyl propyl ester, 6.25g
Acrylic acid and 0.1g polyethylene glycol dimethacrylate are dissolved in methanol, and magnetic agitation is uniformly mixed, and lead to nitrogen half an hour,
The oxygen in mixed solution is removed, mixed solution is obtained；
(3) 0.20g dimethoxybenzoin is dissolved in 2g methanol again, is uniformly mixed；
(4) it after quickly mixing the mixed solution that step (2) obtains with methanol solution in step (3), is uniformly coated on
Step (1) dry after aramid fabric net surface, lead to nitrogen half an hour, remove oxygen；
It at (5) 25 DEG C, is reacted 18 hours under the ultraviolet light of 365nm, forms organic gel layer in fabric surface；
(6) it is immersed in distilled water 48 hours, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.
Fluorine-containing aquagel membrane prepared by the above method detects its contact angle, the contact angle to water is 40 °, to just
The contact angle of hexane oil droplet is 100 °, and 20 ° of roll angle, aperture is 20-25 μm.
It uses the steel wire of 100 mesh as support above-mentioned fluorine-containing aquagel membrane, carries out oil using Simple oil-water separator
Water separating experiment, by the mixture of preprepared n-hexane and water (volume ratio 4: 7, magnetic agitation 30 minutes, oil droplet size
30-35 μm) it is poured on fluorine-containing aquagel membrane, under the pressure less than 0.04MPa, water passes through fluorine-containing aquagel membrane and flows from below
Out, while n-hexane is blocked in the top of fluorine-containing aquagel membrane, but contains part n-hexane in water, and separative efficiency is
70%, separating effect is unobvious.
To sum up, the present invention provides a kind of preparation method and application of hydrophilic and oleophobic fluorine-containing aquagel membrane, this method operation
Simply, it is easy to large scale preparation, manufactured fluorine-containing aquagel membrane intensity is high and at low cost, carries out the high-efficient of water-oil separating.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of fluorine-containing aquagel membrane characterized by comprising
(1) fabric is immersed in acetone and is carried out ultrasound 30 minutes, after cleaning up, dried at normal temperature；
(2) at 5-40 DEG C, acrylate containing fluorine monomer, hydrophilic monomer, crosslinking agent and reducing agent are dissolved in methanol simultaneously
It stirs evenly, leads to the oxygen in nitrogen removing mixed solution, obtain mixed solution；
(3) oxidant is dissolved in methanol；
(4) mixed solution that step (2) obtains quickly is mixed with aqueous solution in step (3), is uniformly coated on step (1) and dries in the air
Then the surface of fabric after dry leads to nitrogen and removes oxygen；
(5) 10-30 minutes are stood at 5-40 DEG C, makes acrylate containing fluorine monomer and hydrophilic monomer in redox initiator
Under the action of carry out polymerisation in solution, form organic gel layer in fabric surface；
(6) it is immersed in distilled water 12-96 hours, removes methanol, obtain hydrophilic and oleophobic fluorine-containing aquagel membrane.
2. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that in the step (1), fabric
For the nylon of 150-300 mesh, polyvinyl, aramid fiber, terylene or acrylic fiber fabric.
3. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that fluorine-containing in the step (2)
Acrylic ester monomer is trifluoroethyl methacrylate, tetrafluoropropyl propyl ester, Hexafluorobutyl mathacrylate, methyl
One of perfluoroethyl butyl ethyl ester, dodecafluoroheptyl methacrylate, methacrylic acid perfluoro hexyl ethyl ester or
It is a variety of.
4. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that hydrophilic in the step (2)
Property monomer be one of acrylamide, acrylic acid, sodium acrylate, potassium acrylate, polyalkylene glycol acrylate or a variety of.
5. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that in the step (2), crosslinking
Agent is one of N, N '-methylene-bisacrylamide, polyethylene glycol dimethacrylate, ethylene glycol dimethacrylate
Or it is a variety of.
6. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that in the step (2), reduction
Agent is N, N- dimethyl-p-toluidine or n,N-Dimethylaniline.
7. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that in the step (2), mixing
The content of acrylate containing fluorine monomer is 1-10wt% in object, and the content of hydrophilic monomer is 20-30wt%；Crosslinking agent contains
Amount is 0.2-0.8wt%, the content of oxidant is 0.4-0.8wt%, and the content of reducing agent is 0.1-0.4wt%, and surplus is first
Alcohol.
8. the preparation method of fluorine-containing aquagel membrane according to claim 1, which is characterized in that in the step (3), oxidation
Agent is benzoyl peroxide, cyclohexanone peroxide, methyl ethyl ketone peroxide or diphenyl peroxide first phthalein.
9. the preparation method of -8 any fluorine-containing aquagel membranes according to claim 1, which is characterized in that the fluorinated water of preparation
Gel mould is lower than 40 ° to the contact angle of water droplet, is greater than 120 ° to the contact angle of oil droplet, roll angle is lower than 25 °, and alcohol content is greater than
85%.
10. the application of the fluorine-containing aquagel membrane of the preparation method preparation of any fluorine-containing aquagel membrane of claim 1-9,
It is characterized in that, the separation for oily wastewater and oil-in-water emulsion.
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| CN110079059A (en) * | 2019-03-28 | 2019-08-02 | 桐乡珠力高分子材料科技有限公司 | Polyester master particle of hydrophilic soil release and preparation method thereof |
| CN110172123A (en) * | 2019-05-27 | 2019-08-27 | 苏州大学 | Hydrophilic and oleophobic property porous polymer and preparation method thereof |
| CN114405287A (en) * | 2022-01-24 | 2022-04-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Superstrong oil stain resistance oil-water separation membrane and preparation method and application thereof |
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