CN106474933A - The preparation method of hollow fiber ultrafiltration membrane - Google Patents
The preparation method of hollow fiber ultrafiltration membrane Download PDFInfo
- Publication number
- CN106474933A CN106474933A CN201610964589.6A CN201610964589A CN106474933A CN 106474933 A CN106474933 A CN 106474933A CN 201610964589 A CN201610964589 A CN 201610964589A CN 106474933 A CN106474933 A CN 106474933A
- Authority
- CN
- China
- Prior art keywords
- solution
- support tube
- basic unit
- aqueous phase
- syringe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- B01D67/0006—Organic membrane manufacture by chemical reactions
-
- 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
- B01D69/08—Hollow fibre membranes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to the preparation method of hollow fiber ultrafiltration membrane, can effectively solving prior art produce ultrafilter membrane poor mechanical property, hydrophilic and water penetration decline, cannot meet in commercial production and problem is actually needed to ultrafilter membrane, method is, dissolve a polymer in solvent, uniform stirring, obtain the solution of polymer；Polymer solution is injected in spinning syringe, uniformly it is wrapped in the outer surface of support tube, become and support tube outer surface to have the nanofiber basic unit of supermembrane, then rinsed with ionized water, it is dried, it is then immersed in aqueous phase monomers solution carrying out interface polymerization reaction, takes out, remove top layer liquid, immerse organic faciess monomer solution again to take out, blot outer surface liquid, carry out heat treatment, become hollow fiber ultrafiltration membrane；Scientific formula of the present invention, abundant raw material, method is simple, easy to operate, good product quality, and mechanical property is strong, hydrophilic and good water permeability, and production efficiency is high, has good economic and social benefit.
Description
Technical field
The present invention relates to chemical industry, particularly a kind of preparation method of hollow fiber ultrafiltration membrane.
Background technology
In contemporary industry produces, ultrafilter membrane is conventional filtration applications, and membrane separation technique is new, efficient point of the present age
From technology, modern industry energy-conservation, improve production efficiency, the recycling of raw material and the need eliminating the aspects such as environmental pollution can be met
Will.Ultrafilter membrane be one kind between micro-filtration membrane and NF membrane with pressure-actuated film, the commercial Application of ultrafilter membrane is very wide
General, it has also become one of novel chemical unit operation, can be used for separation, concentration, purifying biological product, pharmaceutical products and food work
In industry；It is additionally operable to the terminal processing device in blood treatment, wastewater treatment and ultra-pure water preparation.Most of at present business-like super
Filter membrane is using the preparation of submergence inversion of phases, but due to problem present on preparation method, the poor mechanical property of ultrafilter membrane, Jing Guoshi
Answering property processes the ultrafilter membrane of mechanics better performances, and its hydrophilic and water penetration have significantly decline it is impossible to meet industry life
In product, ultrafilter membrane is actually needed.Therefore, the improvement on ultrafiltration membrane preparation method and innovation are imperative.
Content of the invention
For above-mentioned situation, for overcoming the defect of prior art, the purpose of the present invention is exactly to provide a kind of doughnut to surpass
The preparation method of filter membrane, effectively solving prior art can produce the poor mechanical property of ultrafilter membrane, hydrophilic and water penetration decline, no
Method meets in commercial production and to be actually needed problem to ultrafilter membrane.
The technical scheme that the present invention solves also provides a kind of preparation method of hollow fiber ultrafiltration membrane, comprises the following steps：
The first step：In the outer surface of support tube, coated with nano fibrous base layers are prepared by electrostatic spinning process；
Wherein, the hollow fiber ultrafiltration membrane that the present invention provides, including inner liner support pipe, nanofiber basic unit and ultra-filtration and separation
Layer；The external diameter of described support tube is 1.0-2.3mm, and wall thickness is 0.1-0.7mm；Described nanofiber basic unit in support tube and divides
Between absciss layer；
The material of described support tube is polyethylene terephthalate, polyamide, poly(isophthaloyl metaphenylene diamine), polychlorostyrene second
Alkene, polyurethanes, polypropylene are fine, group more than one or more of polypropylene, polyethylene and polyvinyl formal
Close；
The material of described nanofiber basic unit be one or more of polyether sulfone, polysulfones, Hemerocallis citrina Baroni polyether sulfone or polyvinyl alcohol with
On combination；
Nanofiber basic unit is prepared by electrostatic spinning process, comprises the following steps：
A1：Selective polymer（One or more of polyether sulfone, polysulfones, Hemerocallis citrina Baroni polyether sulfone or polyvinyl alcohol）, polymer is molten
Solution, in solvent, is stirring uniformly to obtain melt or the solution of polymer, and its concentration range is 5wt%-50wt%；
Described solvent is the solvent of the close polymer of dissolving, described solvent is DMF, normal heptane, dichloromethane,
Chloroform, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide, glycerol, ethylene glycol, Polyethylene Glycol, dimethyl are sub-
The combination of one or more of sulfone, phenol, amide-type；
A2：Polymer spinning solution is injected in spinning syringe, basic unit, described pin are prepared using syringe needle electrospinning device
The running voltage of head electrospinning device is 10-90KV, and the distance of described syringe to described catcher is 5-50cm；
A3：When using syringe needle electrospinning device, syringe needle is fixed and is evenly distributed on the outer ring of cylinder catcher；Meanwhile, prop up
Stay tube is evenly spaced in the outer ring of cylinder type catcher, and rolls catcher synchronous rotary and presses setting speed advance, and supports
Pipe does not carry out spinning motion, and nanofiber is uniformly wrapped in the outer surface of support tube.
Second step：By the above-mentioned support tube being coated with nanofiber basic unit, carry out standby after ionized water rinses and is dried；
3rd step：By the support tube immersion aqueous phase monomers solution after above-mentioned second step is processed, then it is molten to immerse organic faciess monomer
Carry out interface polymerization reaction in liquid；Can get the hollow fiber ultrafiltration membrane of the present invention.
The preparation method of hollow fiber ultrafiltration membrane of the present invention comprises the following steps that：
（1）, in the outer surface of support tube, nanofiber basic unit is prepared by electrostatic spinning process；
It is formulated for preparing the polymer solution of nanofiber basic unit：Dissolve a polymer in solvent, uniform stirring, is polymerized
The solution of thing（Or title solution）, its weight concentration is 5-50%；
Described polymer is one of polyether sulfone, polysulfones, Hemerocallis citrina Baroni polyether sulfone or polyvinyl alcohol or two or more compositionss；
Described solvent is the N-Methyl pyrrolidone of the close polymer of dissolving, N,N-dimethylformamide, normal heptane, dichloromethane,
Chloroform, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide, glycerol, ethylene glycol, Polyethylene Glycol, dimethyl are sub-
One of sulfone, phenol, amide-type or two or more mixture；
After prepared polymer solution, need to add 4 hydroxybutyric acid into polymer solution；4 hydroxybutyric acid and the matter of polymer
Amount ratio is 1：20.
The polymer solution obtaining is injected in spinning syringe, outer in support tube using syringe needle electrospinning device
Nanofiber basic unit is prepared on surface, and syringe needle is fixed and is evenly distributed on the outer ring of cylinder catcher, and support tube is evenly spaced in rolling
The outer ring of cartridge type catcher, and rolls catcher synchronous rotary and presses setting speed advance, and support tube do not carry out spinning motion, receive
Rice fiber is uniformly wrapped in the outer surface of support tube, becomes to support tube outer surface to have the nanofiber basic unit of supermembrane；
Described support tube external diameter is 1.0-2.3mm, wall thickness 0.1-0.7mm；The material of described support tube is poly terephthalic acid
Glycol ester, polyamide, poly(isophthaloyl metaphenylene diamine), polrvinyl chloride, polyurethanes, polypropylene are fine, polypropylene, poly-
Combination more than one or more of ethylene and polyvinyl formal；
The running voltage of described syringe needle electrospinning device is 10～90KV, and the distance of described syringe to described catcher is 5
～50cm；
（2）, cleaning：By step（1）The nanofiber basic unit made ionized water rinses 20s, places dry in 40-90 DEG C of environment
Dry to dry；
（3）, by step（2）The support tube being enclosed with nanofiber basic unit after cleaning-drying is immersed in 20-25 DEG C of aqueous phase monomers
Carry out interface polymerization reaction 30～180s in solution, take out, remove top layer liquid, be then immersed in 20～25 DEG C of organic faciess monomer
Solution 60～300s takes out, and blots outer surface liquid, then carries out heat treatment 5～30min, Cheng Zhong in 60～120 DEG C of environment
Fibre ultrafiltration film；
Except having directly and in addition to acyl chlorides monomer generation polyamine monomers in described aqueous phase monomers solution, it is also added with acid absorbent hydrogen-oxygen
Change sodium, volume ratio is the surfactant sodium dodecyl base sodium sulfonate of 0.04-0.08%；
Described aqueous phase monomers are m-diaminobenzene., p-phenylenediamine, o-phenylenediamine, equal benzene triamine, 4- methylresorcinol diamidogen, isophthalic two
Amine -5- sulfonic acid, piperazine, one of Isosorbide-5-Nitrae-cyclohexanediamine or two or more mixture；
Described organic faciess monomer is paraphthaloyl chloride, m-phthaloyl chloride, o-phthaloyl chloride, pyromellitic trimethylsilyl chloride, 1,3,
One of 5- cyclohexane three formyl chloride and 1,3,4- Pentamethylene. three acyl chlorides or two or more mixture.
Scientific formula of the present invention, abundant raw material, method is simple, easy to operate, good product quality, and mechanical property is strong, hydrophilic
And good water permeability, production efficiency height, there is good economic and social benefit.
Specific embodiment
With reference to embodiments the specific embodiment of the present invention is elaborated.
The present invention is given by following examples in being embodied as.
Embodiment 1
The present invention, in being embodied as, comprises the following steps：
（1）, in the outer surface of support tube, nanofiber basic unit is prepared by electrostatic spinning process；
It is formulated for preparing the polymer solution of nanofiber basic unit；Dissolve a polymer in solvent, uniform stirring, is polymerized
The solution of thing, its weight concentration is 5-50%；
Described polymer is one of polyether sulfone, polysulfones, Hemerocallis citrina Baroni polyether sulfone or polyvinyl alcohol or two or more compositionss；
Described solvent is the N-Methyl pyrrolidone of the close polymer of dissolving, N,N-dimethylformamide, normal heptane, dichloromethane,
Chloroform, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide, glycerol, ethylene glycol, Polyethylene Glycol, dimethyl are sub-
One of sulfone, phenol, amide-type or two or more mixture；After prepared polymer solution, need into polymer solution
Add 4 hydroxybutyric acid；4 hydroxybutyric acid is 1 with the mass ratio of polymer：20.
The polymer solution obtaining is injected in spinning syringe, outer in support tube using syringe needle electrospinning device
Nanofiber basic unit is prepared on surface, and syringe needle is fixed and is evenly distributed on the outer ring of cylinder catcher, and support tube is evenly spaced in rolling
The outer ring of cartridge type catcher, and rolls catcher synchronous rotary and presses setting speed advance, and support tube do not carry out spinning motion, receive
Rice fiber is uniformly wrapped in the outer surface of support tube, becomes to support tube outer surface to have the nanofiber basic unit of supermembrane；Described pin
The running voltage of head electrospinning device is 10～90KV, and the distance of described syringe to described catcher is 5～50cm.
Described support tube external diameter is 1.0-2.3mm, wall thickness 0.1-0.7mm；The material of described support tube is poly- to benzene two
Formic acid glycol ester, polyamide, poly(isophthaloyl metaphenylene diamine), polrvinyl chloride, polyurethanes, polypropylene are fine, poly- third
Combination more than one or more of alkene, polyethylene and polyvinyl formal；
（2）, cleaning：By step（1）The nanofiber basic unit made ionized water rinses 20s, places dry in 40-90 DEG C of environment
Dry to dry；
（3）, by step（2）The support tube being enclosed with nanofiber basic unit after cleaning-drying is immersed in 20-25 DEG C of aqueous phase monomers
Carry out interface polymerization reaction 30～180s in solution, take out, remove top layer liquid, be then immersed in 20～25 DEG C of organic faciess monomer
Solution 60～300s takes out, and blots outer surface liquid, then carries out heat treatment 5～30min, cost in 60～120 DEG C of environment
Inventive embodiments hollow fiber ultrafiltration membrane；
It is also added with the surfactant sodium dodecyl base sodium sulfonate that volume ratio is 0.04-0.08% in described aqueous phase monomers solution；
Described aqueous phase monomers are m-diaminobenzene., p-phenylenediamine, o-phenylenediamine, equal benzene triamine, 4- methylresorcinol diamidogen, isophthalic two
Amine -5- sulfonic acid, piperazine, one of Isosorbide-5-Nitrae-cyclohexanediamine or two or more mixture；
Described organic faciess monomer is paraphthaloyl chloride, m-phthaloyl chloride, o-phthaloyl chloride, pyromellitic trimethylsilyl chloride, 1,3,
One of 5- cyclohexane three formyl chloride and 1,3,4- Pentamethylene. three acyl chlorides or two or more mixture.
Embodiment 2
The present invention, in being embodied as, comprises the following steps：
（1）It is formulated for preparing the polymer solution of nanofiber basic unit；20g polysulfones is dissolved in 200ml N- crassitude
In ketone, add the polysulfones homogeneous solution that 1g 4 hydroxybutyric acid obtains 10%；
Solution is added in syringe, using syringe needle electrospinning device support tube outer surface prepare nanofiber-based
Layer；Described syringe sets and pushes away speed is 7 μ l/min, the golden Rotation of receiver cylinder 8cm of syringe distance, support tube be longitudinally travelled speed
Spend for 5cm/min；
（2）20s is rinsed with ionized water in the nanofiber obtaining basic unit, is positioned over 40 DEG C of the indoor 1h that is dried afterwards, stand-by.
（3）Will be through above-mentioned（2）Support tube immersion aqueous phase monomers solution after process；
Prepare aqueous phase solution：It is in 9.5 about the solution containing dodecyl sodium sulfate that piperazine is dissolved in pH value, and piperazine concentration is
0.10 (w/v) %, dodecyl sodium sulfate concentration 0.06 (w/v) %.Support tube after step 2 is processed is immersed 20～25 DEG C
Aqueous phase monomers solution in 120s, remove top layer liquid after taking-up；
Immerse organic phase solution again；Prepare organic phase solution：Pyromellitic trimethylsilyl chloride is dissolved in normal hexane so as to concentration is 0.25
(w/v)%；React 60s by removing in the support tube immersion organic faciess after excess surface moisture；Rinsed well with normal hexane, drip
Dry, rinsed with pure water.
Embodiment 3
The present invention, in being embodied as, comprises the following steps：
（1）It is formulated for preparing the polymer solution of nanofiber basic unit；20g polyether sulfone is dissolved in 200ml N- methylpyrrole
In alkanone, add the polysulfones homogeneous solution that 1g 4 hydroxybutyric acid obtains 10%；Solution is added in syringe, described injection
Device sets and pushes away speed is 7 μ l/min, the golden Rotation of receiver cylinder 8cm of syringe distance, and the speed that is longitudinally travelled of support tube is 5cm/
min；
（2）20s is rinsed with ionized water in the porous obtaining basic unit, is positioned over 40 DEG C of the indoor 1h that is dried afterwards, stand-by.
（3）Will be through above-mentioned（2）Support tube immersion aqueous phase monomers solution after process；
Prepare aqueous phase solution；It is isophthalic two in 9.5 about the solution containing dodecyl sodium sulfate that m-diaminobenzene. is dissolved in pH value
Amine concentration is 0.05 (w/v) %, dodecyl sodium sulfate concentration 0.06 (w/v) %；By the support tube immersion after step 2 is processed
120s in 20～25 DEG C of aqueous phase monomers solution, removes top layer liquid after taking-up；
Immerse organic phase solution again；Prepare organic phase solution：Pyromellitic trimethylsilyl chloride is dissolved in normal hexane so as to concentration is 0.1
(w/v)%.60s will be reacted in support tube immersion organic faciess after above-mentioned removing excess surface moisture；Rinsed well with normal hexane,
Drain, rinsed with pure water.
Embodiment 4
The present invention, in being embodied as, comprises the following steps：
（1）It is formulated for preparing the polymer solution of nanofiber basic unit；
20g sulfonated polyether sulfone is dissolved in 200ml N-Methyl pyrrolidone, add 1g 4 hydroxybutyric acid obtain 10% poly-
Sulfone homogeneous solution.Solution is added in syringe, described syringe sets and pushes away speed is 7 μ l/min, the golden rotation of syringe distance
Turn receiving barrel 8cm, the speed that is longitudinally travelled of support tube is 5cm/min；
（2）20s is rinsed with ionized water in the porous obtaining basic unit, is positioned over 40 DEG C of the indoor 1h that is dried afterwards, stand-by.
（3）Will be through above-mentioned（2）Support tube immersion aqueous phase monomers solution after process；
Prepare aqueous phase solution：It is in 9.5 about the solution containing dodecyl sodium sulfate that piperazine is dissolved in pH value, and piperazine concentration is
0.10 (w/v) %, dodecyl sodium sulfate concentration 0.06 (w/v) %；Support tube after step 2 is processed is immersed 20～25 DEG C
Aqueous phase monomers solution in 90s, remove top layer liquid after taking-up；
Immerse organic phase solution again；Prepare organic phase solution：Phthalyl chloride is dissolved in normal hexane so as to concentration is 0.3 (w/
v)%.60s will be reacted in support tube immersion organic faciess after above-mentioned removing excess surface moisture；Rinsed well with normal hexane, drip
Dry, rinsed with pure water.
Through applying on the spot and testing, hollow fiber ultrafiltration membrane has strong mechanical performance, hydrophilic and water penetration to the present invention, should
Preparation method process is simple and production efficiency height, effective for separation, concentration, purifying biological product, pharmaceutical products and food
In industry；It is additionally operable to the terminal processes in blood treatment, wastewater treatment and ultra-pure water preparation, wide application, production efficiency improves
More than 30%, cost reduction does not result in pollution, energy-conserving and environment-protective to environment in more than 1/3, and production process, has good economy
And social benefit.
Claims (6)
1. a kind of preparation method of hollow fiber ultrafiltration membrane is it is characterised in that comprise the following steps：
（1）, in the outer surface of support tube, nanofiber basic unit is prepared by electrostatic spinning process；
It is formulated for preparing the polymer solution of nanofiber basic unit；Dissolve a polymer in solvent, uniform stirring, is polymerized
The solution of thing, its weight concentration is 5-50%；
Described polymer is one of polyether sulfone, polysulfones, Hemerocallis citrina Baroni polyether sulfone or polyvinyl alcohol or two or more compositionss；
Described solvent is the N-Methyl pyrrolidone of the close polymer of dissolving, N,N-dimethylformamide, normal heptane, dichloromethane,
Chloroform, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide, glycerol, ethylene glycol, Polyethylene Glycol, dimethyl are sub-
One of sulfone, phenol, amide-type or two or more mixture；
The polymer solution obtaining is injected in spinning syringe, using syringe needle electrospinning device support tube outer surface
Prepare nanofiber basic unit, syringe needle is fixed and is evenly distributed on the outer ring of cylinder catcher, and support tube is evenly spaced in cylinder type
The outer ring of catcher, and rolls catcher synchronous rotary and presses setting speed advance, and support tube do not carry out spinning motion, Nanowire
Dimension is uniformly wrapped in the outer surface of support tube, becomes to support tube outer surface to have the nanofiber basic unit of supermembrane；
Described support tube external diameter is 1.0-2.3mm, wall thickness 0.1-0.7mm；The material of described support tube is poly terephthalic acid
Glycol ester, polyamide, poly(isophthaloyl metaphenylene diamine), polrvinyl chloride, polyurethanes, polypropylene are fine, polypropylene, poly-
Combination more than one or more of ethylene and polyvinyl formal；
（2）, cleaning：By step（1）The nanofiber basic unit made ionized water rinses 20s, places dry in 40-90 DEG C of environment
Dry to dry；
（3）, by step（2）The support tube being enclosed with nanofiber basic unit after cleaning-drying is immersed in 20-25 DEG C of aqueous phase monomers
Carry out interface polymerization reaction 30～180s in solution, take out, remove top layer liquid, be then immersed in 20～25 DEG C of organic faciess monomer
Solution 60～300s takes out, and blots outer surface liquid, then carries out heat treatment 5～30min, Cheng Zhong in 60～120 DEG C of environment
Fibre ultrafiltration film；
It is also added with the surfactant sodium dodecyl base sodium sulfonate that volume ratio is 0.04-0.08% in described aqueous phase monomers solution；
Described aqueous phase monomers are m-diaminobenzene., p-phenylenediamine, o-phenylenediamine, equal benzene triamine, 4- methylresorcinol diamidogen, isophthalic two
Amine -5- sulfonic acid, piperazine, one of Isosorbide-5-Nitrae-cyclohexanediamine or two or more mixture；
Described organic faciess monomer is paraphthaloyl chloride, m-phthaloyl chloride, o-phthaloyl chloride, pyromellitic trimethylsilyl chloride, 1,3,
One of 5- cyclohexane three formyl chloride and 1,3,4- Pentamethylene. three acyl chlorides or two or more mixture.
2. the preparation method of hollow fiber ultrafiltration membrane according to claim 1 is it is characterised in that described syringe needle electrostatic spinning
The running voltage of equipment is 10～90KV, and the distance of described syringe to described catcher is 5～50cm.
3. the preparation method of hollow fiber ultrafiltration membrane according to claim 1 is it is characterised in that described（1）In, prepare poly-
After polymer solution, need to add 4 hydroxybutyric acid into polymer solution；4 hydroxybutyric acid is 1 with the mass ratio of polymer：20.
4. the preparation method of hollow fiber ultrafiltration membrane according to claim 1 is it is characterised in that comprise the following steps：
（1）It is formulated for preparing the polymer solution of nanofiber basic unit；20g polysulfones is dissolved in 200ml N- crassitude
In ketone, add the polysulfones homogeneous solution that 1g 4 hydroxybutyric acid obtains 10%；
Solution is added in syringe, using syringe needle electrospinning device support tube outer surface prepare nanofiber-based
Layer；Described syringe sets and pushes away speed is 7 μ l/min, the golden Rotation of receiver cylinder 8cm of syringe distance, support tube be longitudinally travelled speed
Spend for 5cm/min；
（2）20s is rinsed with ionized water in the nanofiber obtaining basic unit, is positioned over 40 DEG C of the indoor 1h that is dried afterwards, stand-by；
（3）Will be through above-mentioned（2）Support tube immersion aqueous phase monomers solution after process；
Prepare aqueous phase solution：It is in 9.5 about the solution containing dodecyl sodium sulfate that piperazine is dissolved in pH value, and piperazine concentration is
0.10 (w/v) %, dodecyl sodium sulfate concentration 0.06 (w/v) %, the support tube after step 2 is processed is immersed 20～25 DEG C
Aqueous phase monomers solution in 120s, remove top layer liquid after taking-up；
Immerse organic phase solution again；Prepare organic phase solution：Pyromellitic trimethylsilyl chloride is dissolved in normal hexane so as to concentration is 0.25
(w/v)%；React 60s by removing in the support tube immersion organic faciess after excess surface moisture；Rinsed well with normal hexane, drip
Dry, rinsed with pure water.
5. the preparation method of hollow fiber ultrafiltration membrane according to claim 1 is it is characterised in that comprise the following steps：
（1）It is formulated for preparing the polymer solution of nanofiber basic unit；20g polyether sulfone is dissolved in 200ml N- methylpyrrole
In alkanone, add the polysulfones homogeneous solution that 1g 4 hydroxybutyric acid obtains 10%；Solution is added in syringe, described injection
Device sets and pushes away speed is 7 μ l/min, the golden Rotation of receiver cylinder 8cm of syringe distance, and the speed that is longitudinally travelled of support tube is 5cm/
min；
（2）20s is rinsed with ionized water in the porous obtaining basic unit, is positioned over 40 DEG C of the indoor 1h that is dried afterwards, stand-by；
（3）Will be through above-mentioned（2）Support tube immersion aqueous phase monomers solution after process；
Prepare aqueous phase solution；It is isophthalic two in 9.5 about the solution containing dodecyl sodium sulfate that m-diaminobenzene. is dissolved in pH value
Amine concentration is 0.05 (w/v) %, dodecyl sodium sulfate concentration 0.06 (w/v) %；By the support tube immersion after step 2 is processed
120s in 20～25 DEG C of aqueous phase monomers solution, removes top layer liquid after taking-up；
Immerse organic phase solution again；Prepare organic phase solution：Pyromellitic trimethylsilyl chloride is dissolved in normal hexane so as to concentration is 0.1
(w/v) %, will react 60s in the support tube immersion organic faciess after above-mentioned removing excess surface moisture；Rinsed well with normal hexane,
Drain, rinsed with pure water.
6. the preparation method of hollow fiber ultrafiltration membrane according to claim 1 is it is characterised in that comprise the following steps：
It is formulated for preparing the polymer solution of nanofiber basic unit；
20g sulfonated polyether sulfone is dissolved in 200ml N-Methyl pyrrolidone, add 1g 4 hydroxybutyric acid obtain 10% poly-
Sulfone homogeneous solution, solution is added in syringe, and described syringe sets and pushes away speed is 7 μ l/min, the golden rotation of syringe distance
Turn receiving barrel 8cm, the speed that is longitudinally travelled of support tube is 5cm/min；
（2）20s is rinsed with ionized water in the porous obtaining basic unit, is positioned over 40 DEG C of the indoor 1h that is dried afterwards, stand-by；
（3）Will be through above-mentioned（2）Support tube immersion aqueous phase monomers solution after process；
Prepare aqueous phase solution：It is in 9.5 about the solution containing dodecyl sodium sulfate that piperazine is dissolved in pH value, and piperazine concentration is
0.10 (w/v) %, dodecyl sodium sulfate concentration 0.06 (w/v) %；Support tube after step 2 is processed is immersed 20～25 DEG C
Aqueous phase monomers solution in 90s, remove top layer liquid after taking-up；
Immerse organic phase solution again；Prepare organic phase solution：Phthalyl chloride is dissolved in normal hexane so as to concentration is 0.3 (w/
V) %, will react 60s in the support tube immersion organic faciess after above-mentioned removing excess surface moisture；Rinsed well with normal hexane, drip
Dry, rinsed with pure water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610964589.6A CN106474933A (en) | 2016-10-28 | 2016-10-28 | The preparation method of hollow fiber ultrafiltration membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610964589.6A CN106474933A (en) | 2016-10-28 | 2016-10-28 | The preparation method of hollow fiber ultrafiltration membrane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106474933A true CN106474933A (en) | 2017-03-08 |
Family
ID=58272028
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610964589.6A Pending CN106474933A (en) | 2016-10-28 | 2016-10-28 | The preparation method of hollow fiber ultrafiltration membrane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106474933A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109847595A (en) * | 2018-12-21 | 2019-06-07 | 三达膜科技（厦门）有限公司 | A kind of preparation method of the big compound polyvinylidene fluoride hollow fiber ultrafiltration membrane of flux inner support |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101947415A (en) * | 2010-08-13 | 2011-01-19 | 东华大学 | Combination of electrostatic spinning and electrostatic spraying for preparing nanofibre base composite separation membrane |
| CN102814126A (en) * | 2011-06-09 | 2012-12-12 | 中国科学院城市环境研究所 | Preparation method of high-flux antioxidant nanofiltration membrane |
| CN105169972A (en) * | 2015-09-30 | 2015-12-23 | 北京新源国能科技有限公司 | Hollow fiber nanofiltration membrane and preparation method for producing hollow fiber nanofiltration membrane |
| CN105233708A (en) * | 2015-09-30 | 2016-01-13 | 北京新源国能科技有限公司 | Hollow fiber nano filter membrane and equipment for producing same |
-
2016
- 2016-10-28 CN CN201610964589.6A patent/CN106474933A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101947415A (en) * | 2010-08-13 | 2011-01-19 | 东华大学 | Combination of electrostatic spinning and electrostatic spraying for preparing nanofibre base composite separation membrane |
| CN102814126A (en) * | 2011-06-09 | 2012-12-12 | 中国科学院城市环境研究所 | Preparation method of high-flux antioxidant nanofiltration membrane |
| CN105169972A (en) * | 2015-09-30 | 2015-12-23 | 北京新源国能科技有限公司 | Hollow fiber nanofiltration membrane and preparation method for producing hollow fiber nanofiltration membrane |
| CN105233708A (en) * | 2015-09-30 | 2016-01-13 | 北京新源国能科技有限公司 | Hollow fiber nano filter membrane and equipment for producing same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109847595A (en) * | 2018-12-21 | 2019-06-07 | 三达膜科技（厦门）有限公司 | A kind of preparation method of the big compound polyvinylidene fluoride hollow fiber ultrafiltration membrane of flux inner support |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018120476A1 (en) | Supramolecular composite nano-filtration membrane and preparation method therefor and use thereof | |
| CN102836644B (en) | Method for synchronously preparing hollow fiber compound nanofiltration membrane through immersion precipitation phase inversion/interface crosslinking | |
| CN105363350A (en) | Unsymmetrical chlorine-containing polymer-based charged type hollow fiber filtration membrane and preparation method thereof | |
| CN101227968A (en) | Nano composite hollow fiber membrane and method of manufacturing the same | |
| EP2857088B1 (en) | Method for manufacturing a reverse osmosis membrane | |
| JP2014524827A (en) | Reverse osmosis separation membrane | |
| JP5619867B2 (en) | Method for producing enantioselective composite membrane | |
| CN102824859B (en) | Method for preparing hollow fiber nanofiltration membrane by using thermally induced phase separation/interface cross linking synchronization method | |
| CN104722218B (en) | Preparation method for solvent-resistant modified polyetherimide nanofiltration membrane | |
| CN104174299A (en) | High-flux positive osmosis membrane based on ultrathin support layer and preparation method thereof | |
| CN105934271A (en) | Nanofiltration membrane and method of manufacturing a nanofiltration membrane | |
| CN102258949A (en) | Method for adjusting interfacial structure of polyamide reverse osmosis compound membrane | |
| CN115121128A (en) | Preparation method of composite membrane and composite membrane | |
| CN107638813B (en) | Preparation method and application of hollow fiber solvent-resistant nanofiltration membrane | |
| CN112007513A (en) | Preparation method of meta-aramid-based polyamide composite nanofiltration membrane | |
| CN113230888A (en) | Polyethyleneimine modified nanofiltration membrane and preparation method thereof | |
| CN108452685A (en) | A kind of compound forward osmosis membrane of high-performance and preparation method thereof | |
| CN112516814A (en) | Preparation method of high-desalting solvent-resistant polyamide composite nanofiltration membrane | |
| CN113842783B (en) | Acid-resistant high-flux polyarylether composite nanofiltration membrane, and preparation method and application thereof | |
| CN106890571A (en) | A kind of preparation method of organic tubular nanofiltration membrane | |
| CN102580575A (en) | Method for producing polyvinylidene fluoride membrane for membrane distillation | |
| CN106474933A (en) | The preparation method of hollow fiber ultrafiltration membrane | |
| CN107670504B (en) | A method of the organic tubular nanofiltration membrane of solvent resistant is prepared using bidirectional circulating perfusion | |
| CN110743380B (en) | Preparation method of nanofiltration membrane and nanofiltration membrane prepared by same | |
| CN108211826A (en) | A kind of forward osmosis membrane and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170308 |
|
| RJ01 | Rejection of invention patent application after publication |