CN108479432A - A kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane - Google Patents
A kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/0025—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching
- B01D67/0027—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching by stretching
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- B01D69/08—Hollow fibre membranes
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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
- B01D69/08—Hollow fibre membranes
- B01D69/081—Hollow fibre membranes characterised by the fibre diameter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
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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
- B01D2325/22—Thermal or heat-resistance properties
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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
- B01D2325/30—Chemical resistance
Abstract
The present invention relates to a kind of preparation methods of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane, including：In organic solvent by phenolphthalein polyether sulfone PES C dissolving, obtain spinning solution, solution jet spinning is dry, obtains PES C nano tunica fibrosas, by crosslinked polyvinylpyrrolidone PVPP solution sprayings in PES C nano fiber film surfaces, hot-pressing processing to get.The present invention prepares composite nano fiber ultrafiltration membrane using solution jet spinning method, compared to the electrostatic spinning technique utilized extensively at present, has the advantages that production efficiency is high, and low energy consumption, and applicable object range is wide, suitable industrialized production；The phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane being prepared has higher hydrophily, thermal stability and acid-alkali-corrosive-resisting, also there is higher contamination resistance, and hydrophily has persistence, it is advantageously implemented industrialized production, and is had broad application prospects in fields such as micro-filtration, ultrafiltration.
Description
Technical field
The invention belongs to modified nano fiber field of membrane preparation, more particularly to a kind of hydrophily phenolphthalein polyether sulfone composite Nano
The preparation method of fiber ultrafiltration membrane.
Background technology
Phenolphthalein polyether sulfone (PES-C) is a kind of novel semi-crystalline state aromatic thermoplastic engineering plastics of China's independent research,
Its glass transition temperature is up to 263 DEG C, heat resisting temperature at 150 DEG C or more, have high-strength and high-modulus, high temperature resistant, endurance, radiation hardness,
Corrosion resistant is lit up and the series of advantages such as good stability of the dimension, is obtained widely in high-tech sectors such as aerospace, electronics, information, the energy
Using.
Phenolphthalein polyether sulfone (PES-C) is a kind of hydrophobic polymer material, therefore in fields such as sewage disposals, in order to overcome
The defects of hydrophobicity and poor contamination resistance of material, it is necessary to which membrane material is modified.Fouling membrane is pollutant in film table
Face and inside deposit and cause the process of membrane flux reduction, research to have shown that hydrophilic surface energy adsorbs more water, Neng Gouyou
The contamination resistance of the raising film of effect, adds hydroaropic substance by modes such as blending, grafting, coatings in hydrophobic film, is
A kind of relatively effective method.
In existing document report, be mostly to by phase inversion or immersion precipitation preparation PES-C ultrafiltration membranes into
Row heat resistance and hydrophilic modification, as CN201110430250 discloses a kind of hydrophily polyethersulfone with cardo alloy ultrafiltration
The preparation method of film, but the hydrophilic modifying for preparing PES-C nanofiber composite hyperfiltration membranes by molten spray spin processes is studied few
It refers to.
Solution jet spinning method has as a kind of novel technology for preparing micro/nano-fibre material compared with electrostatic spinning
Have the advantages that simple for process, low energy consumption, production efficiency is high and safe.Requirement of the solution gunite to equipment is low, preparation side
The simpler convenience of method, it is safe, it is applicable not only to most of polymer material, is also applied for inorganic material, is current
Realize the best mode of nanofiber industrialized production.
Hydrophily cortical material (PVPP) is sprayed to by nanofiber film surface using solution injection apparatus, it is ensured that liquid
Drop can be more uniformly sprayed onto on object, and spray efficiency is high, high to the utilization rate of raw material, and be easy to the thickness of coating
Control, high degree of automation adaptable to the type of spraying, can preferably overcome traditional casting solution to porous basement membrane leakage and
The difficult problem of coating layer thickness control, is conducive to industrialization promotion.
Invention content
Technical problem to be solved by the invention is to provide a kind of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membranes
Preparation method, this method is easy to operate, and low energy consumption, mild condition, be suitble to industrialized production, the phenolphthalein polyether sulfone being prepared
Composite nano fiber ultrafiltration membrane has higher hydrophily, thermal stability and acid-alkali-corrosive-resisting, it may have higher antipollution
Ability is advantageously implemented industrialized production, and has broad application prospects in fields such as micro-filtration, ultrafiltration.
A kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane of the present invention, the specific steps are：
(1) in organic solvent by phenolphthalein polyether sulfone PES-C dissolvings, spinning solution is obtained, solution jet spinning is dry,
Obtain PES-C nano fibrous membranes, the wherein a concentration of 15-35wt% of spinning solution；
(2) by crosslinked polyvinylpyrrolidone PVPP solution sprayings in step (1) PES-C nanofiber film surfaces, heat
Pressure processing, obtains the complete hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane of barrier layer.
Phenolphthalein polyether sulfone PES-C is that (one-step synthesis method carries phthalein side according to patent CN85101721A in the step (1)
The polyether sulphone of base) the method synthesis, method is：The phenolphthalein of 0.02M-0.50M is added in the reactor and waits gram molecules
4,4 '-dichloro diphenyl sulfones add a small amount of toluene and the potassium carbonate more than quantitative relation 5%-100%, and solid content is added and exists
Dimethyl sulfoxide, sulfolane or diphenyl sulphone (DPS) needed for 30%-70% lead to nitrogen protection, first are steamed in temperature-rise period as solvent
Benzene, continue heating polymerize at 170 DEG C -200 DEG C, the time about needs 4-8 hours, when reaching required viscosity, cool down, be added it is molten
Dilution agent is passed through methyl chloride gas closing end group at 100 DEG C or so, and cooled and filtered desalts, down to being precipitated in precipitating reagent, water
It washes, alcohol reflux, it is dry after filtering, obtain white flocculent polymer.
The intrinsic viscosity of the phenolphthalein polyether sulfone PES-C is between 0.4~1.2g/dL, preferably 0.6~0.8g/dL.
Organic solvent is DMF, DMAc or NMP in the step (1).
The technological parameter of solution jet spinning is in the step (1)：Orifice diameter is 0.5~1.0mm, fltting speed
For the holes 1~5ml/h, spinning air pressure is 0.05~0.2MPa, and it is 15~40cm to receive distance, and the spinning time is 1~3h, spinning
Atmosphere used is nitrogen, argon gas or helium.
The preparation method of PVPP solution is in the step (2)：Polyvinylpyrrolidone PVP is soluble in water, obtain PVP
Solution, is added initiator, and crosslinking obtains PVPP solution, wherein a concentration of 1wt%~5wt% of PVP solution, initiator and PVP
Mass ratio be 1:0.5~2.
The molecular weight of the PVP is 1 × 104~130 × 104；Initiator is potassium peroxydisulfate, sodium peroxydisulfate or ammonium persulfate.
The crosslinking temperature is 70~90 DEG C, and crosslinking time is 1h~5h.
Spraying is by solution injection apparatus in the step (2).
The technological parameter of spraying is in the step (2)：Orifice diameter be 0.5~1.0mm, fltting speed be 1~
The holes 5ml/h, spraying air pressure are 0.05~0.2MPa, and it is 15~40cm to receive distance, and spray time is 1~3h, used in spraying
Atmosphere is nitrogen, argon gas or helium.
Hot-pressing processing temperature is 160 DEG C~200 DEG C in the step (2), and hot-pressing processing pressure is 0~10Mpa, and not
It is 0, the hot-pressing processing time is 0~60min, and is not 0.
The present invention is prepared for phenolphthalein polyether sulfone nano fibrous membrane by molten spray spin processes, then cross-linked pvp is sprayed by solution
Injection device is sprayed on barrier layer of the nanofiber film surface as composite membrane, finally again by simple hot-pressing processing, to shape
At a kind of novel permanent hydrophilic, the strong compound PES-C nanofibre hyperfiltration membranes of contamination resistance.The present invention being capable of simple essence
The thickness and uniformity of true control barrier layer, while the hydrophily of notable and lasting raising composite membrane.
The phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane that the present invention obtains can effectively improve the hydrophobic of traditional polysulfones film
Property, PVPP is sprayed into nanofiber film surface by solution injection apparatus, and be simply heat-treated to it.Only need
As soon as fiber film surface adheres to very thin layer PVPP, the hydrophily of film can be dramatically increased.With the extension of spray time, it is attached to
The PVPP of fiber film surface is more and more, although to the hydrophilic beneficial of film, the heat resistance of film can be caused to reduce, improved
The water flux of film can be reduced while rejection, the method is simple for process, practicality and high efficiency, is advantageously implemented industrialization extension and answers
With.
It is traditional using PVP as in the filming technology of additive, since PVP is soluble easily in water, film preparation and after
In continuous filtration application, PVP can all be caused constantly to be lost in the extension of usage time, so that the hydrophily and anti-pollution of material
It contaminates less able.After PVP crosslinkings in the present invention, is ensureing hydrophilic while being no longer dissolve in water and other organic solvents,
The surface that nano fibrous membrane can be more firmly attached to after hot-pressing processing is not easily to fall off, to form a kind of more stable answer
The structure for closing nano fibrous membrane, ensure that the persistence of hydrophilic modifying.
The flux recovery rate (FRR) of film is generally used to indicate the quality of film contamination resistance, and the value is between 0~1, more
Close to 1, show that the contamination resistance of film is stronger.It is defined as follows shown in formula：
Wherein, J0For the initial water flux of film, J is that membrane filtration operation terminates the recovery water flux after cleaning.
Advantageous effect
(1) present invention prepares composite nano fiber ultrafiltration membrane using solution jet spinning method, compared to utilization extensively at present
Electrostatic spinning technique, have production efficiency high, low energy consumption, and applicable object range is wide, the advantages that being suitble to industrialized production；
(2) the phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane being prepared have higher hydrophily, thermal stability and
Acid-alkali-corrosive-resisting, it may have higher contamination resistance, simultaneously because the PVPP for being attached to fiber film surface it is not soluble in water and
Usual vehicle is advantageously implemented industrialized production, can be widely applied to water to ensure that the persistence of hydrophilic modifying effect
Filtering, gas filtration, food processing, medicine, the fields such as purification purifying.
Description of the drawings
Fig. 1 is the solution injection apparatus schematic diagram of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of PES-C nano fibrous membranes in embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of the nanofiber-based composite film surfaces of PES-C in embodiment 1.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
All raw materials are commercial product.
Embodiment 1
(1) the phenolphthalein polyether sulfone of intrinsic viscosity 1.0g/dL is dissolved in DMF, prepares 15wt% spinning solutions, stood de-
Bubble, spinneret pin hole is squeezed out by spinning solution through metering pump, and stretching collection through high-speed flow forms nano fibrous membrane, related work
Skill parameter is：The holes spinning nozzle diameter 0.8mm, fltting speed 5ml/h, spinning air pressure 0.08MPa receive distance 15cm, spinning
Time 2h, atmosphere used in spinning are nitrogen；The dry 10h of 80 DEG C of gained nano fibrous membrane vacuum, obtains PES-C nano fibrous membranes.
(2) solution for preparing PVPK30 5wt% is added potassium peroxydisulfate and is initiator and is 2 with PVPK30 mass ratioes:1,
80 DEG C of reaction 5h of heating, obtain PVPP solution.
(3) PVPP solution in step (2) is sprayed into PES-C nano fibrous membranes in step (1) by solution injection apparatus
Surface, to obtain the compound original nanofibers films of PES-C/PVPP, associated process conditions are：Spinning nozzle diameter 0.5mm, pushes away
Into the holes speed 4ml/h, air pressure 0.05MPa is sprayed, receives distance 25cm, spray time 2h, it is nitrogen to spray atmosphere used, will
Gained composite membrane is immersed in the water removing impurity, the dry 10h of 80 DEG C of vacuum.
(4) gained composite membrane in step (3) is clipped with processing release paper, is put into mold, basement membrane (PES-C) upward, PVPP
Downward, temperature is adjusted to 160 DEG C, pressure 0.5MPa, and processing time is 20min to get PES-C nanofiber group compound films,
PVPP barrier layer thickness is about 7 μm.In certain temperature melt-flow can occur for PVPP to cover entire fiber film surface, and compare
The stronger surface for being attached to nano fibrous membrane is not easily to fall off, and since its crosslinking condition ensures hydrophilic persistence.
The PES-C nanofiber group compound films can be used for ultrafiltration field, and the pure water flux for 50kPa test films of pressurizeing is put down
Mean value is about 320L/m2After h, the ovalbumin solution 1h for then filtering 1g/L, simply rinses several minutes, test again extensive
Rehydration flux is about 282L/m2H, flux recovery rate 88%.
Fig. 2 shows：The other fiber of PES-C micro/nano levels can be prepared by molten spray spin processes, fiber surface is smooth, diameter
It is more uniform, and its spinnability is preferable.
Fig. 3 shows：It by nano fibrous membrane surface spraying PVPP, and carries out after being simply heat-treated, has obtained surface
Uniformly complete PVPP barrier layers.
Embodiment 2
(1) the phenolphthalein polyether sulfone of intrinsic viscosity 0.65g/dL is dissolved in DMF, prepares 25wt% spinning solutions, stood de-
Bubble, spinneret pin hole is squeezed out by spinning solution through metering pump, and stretching collection through high-speed flow forms nano fibrous membrane, related work
Skill parameter is：The holes spinning nozzle diameter 0.7mm, fltting speed 4ml/h, spinning air pressure 0.12MPa receive distance 25cm, spinning
Time 2h, atmosphere used in spinning are nitrogen, and the dry 10h of 80 DEG C of gained nano fibrous membrane vacuum obtains PES-C nano fibrous membranes.
(2) solution for preparing PVPK60 3wt% is added sodium peroxydisulfate and is initiator and is 1 with PVPK60 mass ratioes:1,
70 DEG C of reaction 4h of heating, obtain PVPP solution.
(3) PVPP solution in step (2) is sprayed into nanofiber film surface in step (1) by solution injection apparatus,
To obtain the compound original nanofibers films of PES-C/PVPP, associated process conditions are：Spinning nozzle diameter 0.7mm promotes speed
The holes 3ml/h are spent, air pressure 0.08MPa is sprayed, receive distance 30cm, spray time 1.5h, it is nitrogen to spray atmosphere used, by institute
It obtains composite membrane and is immersed in the water removing impurity, the dry 10h of 80 DEG C of vacuum.
(4) gained composite membrane in step (3) is clipped with processing release paper, is put into mold, basement membrane (PES-C) upward, PVPP
Downward, temperature is adjusted to 180 DEG C, pressure 3MPa, and processing time is 20min to get PES-C nanofiber group compound films,
PVPP barrier layer thickness is about 3 μm.
The PES-C nanofiber group compound films can be used for ultrafiltration field, and the pure water flux for 50kPa test films of pressurizeing is put down
Mean value is about 530L/m2After h, the ovalbumin solution 1h for then filtering 1g/L, simply rinses several minutes, test again extensive
Rehydration flux is about 420L/m2H, flux recovery rate 80%.
Embodiment 3
(1) the phenolphthalein polyether sulfone of intrinsic viscosity 0.5g/dL is dissolved in DMF, prepares 30wt% spinning solutions, stood de-
Bubble, spinneret pin hole is squeezed out by spinning solution through metering pump, and stretching collection through high-speed flow forms nano fibrous membrane, it is related
Technological parameter is：The holes spinning nozzle diameter 0.5mm, fltting speed 5ml/h, spinning air pressure 0.2MPa receive distance 40cm, spinning
Time 2h, atmosphere used in spinning are nitrogen, and the dry 10h of 80 DEG C of gained nano fibrous membrane vacuum obtains PES-C nano fibrous membranes.
(2) solution for preparing PVPK90 2wt% is added ammonium persulfate and is initiator and is 1 with PVPK90 mass ratioes:2,
90 DEG C of reaction 2h of heating, obtain PVPP solution.
(3) PVPP solution in step (2) is sprayed into PES-C nano fibrous membranes in step (1) by solution injection apparatus
Surface, to obtain the compound original nanofibers films of PES-C/PVPP, associated process conditions are：Spinning nozzle diameter 1.0mm, pushes away
Into the holes speed 2.5ml/h, air pressure 0.1MPa is sprayed, receives distance 35cm, spray time 2.5h, it is nitrogen to spray atmosphere used
Gained composite membrane is immersed in the water removing impurity, the dry 10h of 80 DEG C of vacuum by gas.
(4) gained composite membrane in step (3) is clipped with processing release paper, is put into mold, basement membrane (PES-C) upward, PVPP
Downward, temperature is adjusted to 200 DEG C, pressure 1MPa, and processing time is 5min to get PES-C nanofiber group compound films, PVPP
Barrier layer thickness is about 5 μm.
The PES-C nanofiber group compound films can be used for ultrafiltration field, and the pure water flux for 50kPa test films of pressurizeing is put down
Mean value is about 400L/m2After h, the ovalbumin solution 1h for then filtering 1g/L, simply rinses several minutes, test again extensive
Rehydration flux is about 340L/m2H, flux recovery rate 85%.
Embodiment 4
(1) the phenolphthalein polyether sulfone of intrinsic viscosity 0.8g/dL is dissolved in DMF, prepares 20wt% spinning solutions, stood de-
Bubble, spinneret pin hole is squeezed out by spinning solution through metering pump, and stretching collection through high-speed flow forms nano fibrous membrane, it is related
Technological parameter is：The holes spinning nozzle diameter 0.6mm, fltting speed 3ml/h, spinning air pressure 0.15MPa receive distance 30cm, spin
Silk time 2h, atmosphere used in spinning are nitrogen, and the dry 10h of 80 DEG C of gained nano fibrous membrane vacuum obtains PES-C nanofibers
Film.
(2) solution for preparing PVPK30 4wt% is added potassium peroxydisulfate and is initiator and is 1 with PVPK30 mass ratioes:1,
80 DEG C of reaction 5h of heating, obtain PVPP solution.
(3) PVPP solution in step (2) is sprayed into PES-C nano fibrous membranes in step (1) by solution injection apparatus
Surface, to obtain the compound original nanofibers films of PES-C/PVPP, associated process conditions are：Spinning nozzle diameter 0.8mm, pushes away
Into the holes speed 3ml/h, air pressure 0.15MPa is sprayed, receives distance 40cm, spray time 2h, it is nitrogen to spray atmosphere used, will
Gained composite membrane is immersed in the water removing impurity, the dry 10h of 80 DEG C of vacuum.
(4) gained composite membrane in step (3) is clipped with processing release paper, is put into mold, basement membrane (PES-C) upward, PVPP
Downward, temperature is adjusted to 170 DEG C, pressure 2MPa, and processing time is 10min to get PES-C nanofiber group compound films,
PVPP barrier layer thickness is about 6 μm.
The PES-C nanofiber group compound films can be used for ultrafiltration field, and the pure water flux for 50kPa test films of pressurizeing is put down
Mean value is about 350L/m2After h, the ovalbumin solution 1h for then filtering 1g/L, simply rinses several minutes, test again extensive
Rehydration flux is about 315L/m2H, flux recovery rate 90%.
As embodiment as can be seen that may be used on ultrafiltration neck by the composite nano-fiber membrane obtained by barrier layer of PVPP
Domain has preferable anti-protein contamination ability, and large-scale production easy to implement, before having wide application in UF membrane field
Scape.
Claims (8)
1. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane, the specific steps are：
(1) in organic solvent by phenolphthalein polyether sulfone PES-C dissolvings, spinning solution is obtained, solution jet spinning is dry, obtains
PES-C nano fibrous membranes, the wherein a concentration of 15-35wt% of spinning solution；
(2) by crosslinked polyvinylpyrrolidone PVPP solution sprayings in step (1) PES-C nanofiber film surfaces, at hot pressing
Reason, obtains hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane.
2. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane described in accordance with the claim 1,
It is characterized in that, organic solvent is DMF, DMAc or NMP in the step (1).
3. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane described in accordance with the claim 1,
It is characterized in that, the technological parameter of solution jet spinning is in the step (1)：Orifice diameter is 0.5~1.0mm, promotes speed
Degree is the holes 1~5ml/h, and spinning air pressure is 0.05~0.2MPa, and it is 15~40cm to receive distance, and the spinning time is 1~3h, is spun
Atmosphere used in silk is nitrogen, argon gas or helium.
4. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane described in accordance with the claim 1,
It is characterized in that, the preparation method of PVPP solution is in the step (2)：Polyvinylpyrrolidone PVP is soluble in water, it obtains
Initiator is added in PVP solution, and crosslinking obtains PVPP solution, wherein a concentration of 1wt%~5wt% of PVP solution, initiator with
The mass ratio of PVP is 1:0.5~2.
5. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane according to claim 4,
It is characterized in that, the molecular weight of the PVP is 1 × 104~130 × 104；Initiator is potassium peroxydisulfate, sodium peroxydisulfate or persulfuric acid
Ammonium.
6. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane according to claim 4,
It is characterized in that, the crosslinking temperature is 70~90 DEG C, and crosslinking time is 1h~5h.
7. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane described in accordance with the claim 1,
It is characterized in that, the technological parameter sprayed in the step (2) is：Orifice diameter be 0.5~1.0mm, fltting speed be 1~
The holes 5ml/h, spraying air pressure are 0.05~0.2MPa, and it is 15~40cm to receive distance, and spray time is 1~3h, used in spraying
Atmosphere is nitrogen, argon gas or helium.
8. a kind of preparation method of hydrophily phenolphthalein polyether sulfone composite nano fiber ultrafiltration membrane described in accordance with the claim 1,
It being characterized in that, hot-pressing processing temperature is 160 DEG C~200 DEG C in the step (2), and hot-pressing processing pressure is 0~10Mpa, and
It is not 0, the hot-pressing processing time is 0~60min, and is not 0.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113477098A (en) * | 2021-07-08 | 2021-10-08 | 九江学院 | Preparation method of polyarylethersulfone nanofiber-based composite membrane |
| WO2021258701A1 (en) * | 2020-06-23 | 2021-12-30 | 三达膜科技（厦门）有限公司 | Preparation method of sustainable hydrophilic modified polyvinylidene fluoride hollow membrane |
| CN114713038A (en) * | 2022-03-30 | 2022-07-08 | 深圳维度新材料有限公司 | Micro-nano fiber membrane and preparation method and application thereof |
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