CN109224863A - A kind of preparation method of amphipathic modified antipollution polyamide nanofiltration membrane - Google Patents
A kind of preparation method of amphipathic modified antipollution polyamide nanofiltration membrane Download PDFInfo
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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
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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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
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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
- B01D71/26—Polyalkenes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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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
- B01D71/56—Polyamides, e.g. polyester-amides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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Abstract
A kind of preparation method of amphipathic modified polyamide nanofiltration membrane, it proceeds as follows: (1) using ultrafiltration membrane as support membrane, using piperazine as aqueous phase monomers, pyromellitic trimethylsilyl chloride is oil phase monomer, surfactant is water phase additive, active separating layer is formed on ultrafiltration membrane using interfacial polymerization, initial polyamide nanofiltration membrane is made；(2) initial polyamide nanofiltration membrane is fixed with frame, pours into the ethanol solution of configured triethanolamine on its surface, after reacting a period of time, the extra solution of removal film surface dries, obtains hydrophilic modifying nanofiltration membrane；(3) in the film surface of hydrophilic modifying nanofiltration membrane, the ethanol solution of configured perfluoro decyl trichlorosilane is poured into, the extra solution of film surface is removed after reacting a period of time, dries, 60-90 DEG C reaction 5-15 minutes, obtain amphipathic modified polyamide nanofiltration membrane.The method of the present invention is simple, facilitates operation, can react at room temperature, and the amphipathic polyamide nanofiltration membrane of preparation has good antifouling property.
Description
Technical field
The invention belongs to nanofiltration membrane preparation technical fields, and in particular to a kind of amphipathic modified antipollution polyamide nanofiltration membrane
Preparation method.
Background technique
Nanofiltration membrane is pressure drive membrane of the film aperture size in 1nm or so, is existed for divalent ion, relative molecular mass
200~500 organic matter and colloid has very high rejection, and lower to the rejection of monovalent ion.Nanofiltration membrane is wide at present
It is general apply petrochemical industry, pharmacy, environmental protection, food, the energy, electronics, sea water desalination, in terms of.
But in the practical application of nanofiltration membrane, membrane pollution problem be limit membrane process development and application one it is important because
Element.Fouling membrane can block fenestra, make flux depression, reduce the separating property of film, reduce the Acceptable life of film, improve life
The cost of production.For the film polluted, physical cleaning, chemical cleaning and the method removal for more renewing film, but this nothing can be used
The operating cost that will increase membrane separating process is doubted, and palliative.To fundamentally solve the problems, such as this, it is necessary to develop
Novel film materials or current material is modified out, optimizes the structure and performance of film itself, prepare the anti-pollution of function admirable
Contaminate film.
The preparation of resistance tocrocking nanofiltration membrane, it is different by the hydrophilic and hydrophobic of substance used in membrane modifying, three aspects: parent can be divided into
Watersoluble modified, super-hydrophobicity is modified, amphipathic modification.Hydrophilic modifying nanofiltration membrane is intended to improve the hydrophily of film and in film surface shape
At one layer of fine and close hydration layer, to prevent the attachment and blocking of pollutant；The modified nanofiltration film surface of super-hydrophobicity is to hydrone
There is repulsive force, to reduce the touch opportunity of solution and film surface, moreover, super-hydrophobicity film surface has lower surface
Can, even if there is sub-fraction pollutant that can reach film surface, it is also difficult to be attached to above, to reach resistant to pollution effect.
Hydrophilic modifying film by film surface formed hydration layer block contaminant absorption, once but pollutant in pressure
Hydration layer is passed through under effect of dragging and reaches film surface, and pollutant will be deposited on film surface and cause fouling membrane.And self-cleaning surface
The hydrophobicity of low-surface-energy material itself can reduce the water flux of film.Based on deficiency present in both the above method of modifying, together
When have hydrophilic segment and the amphipathic surface of low-surface-energy part and seem particularly necessary: hydrophilic segment be conducive to make film obtain compared with
High water flux and lower flux decline, low-surface-energy part are conducive to weaken the phase interaction between film surface and pollutant
With." pollution defense mechanism " and " pollution releasing mechanism " ingenious combined amphipathic film surface can effectively be prevented more
The absorption and deposition of multiple pollutant.A kind of side for preparing amphipathic modified antipollution polyamide nanofiltration membrane of invention
Method.
Summary of the invention
The purpose of the present invention is to provide it is a kind of simple, facilitate operation, reactive amphipathic amide received at room temperature
The preparation method of filter membrane, the amphipathic polyamide nanofiltration membrane have good antifouling property.
To the present invention, used technical solution is illustrated for achieving the above object below.
The present invention provides a kind of preparation methods of amphipathic modified polyamide nanofiltration membrane, carry out in accordance with the following steps:
(1) preparation of polyamide nanofiltration membrane: using ultrafiltration membrane as support membrane, using piperazine as aqueous phase monomers, equal benzene front three
Acyl chlorides is oil phase monomer, and surfactant is water phase additive, and active separating layer is formed on ultrafiltration membrane using interfacial polymerization,
Initial polyamide nanofiltration membrane is made；The surfactant is dodecyl sodium sulfate, neopelex, tristearin
One or more of acid or ammonium lauryl sulfate；
(2) preparation of hydrophilic modifying nanofiltration membrane: initial polyamide nanofiltration membrane is fixed with frame, is poured into and is matched on its surface
The ethanol solution for the triethanolamine set, after reacting a period of time, the extra solution of removal film surface is dried, is realized with this poly-
The hydrophilic modifying of amide nanofiltration membrane obtains hydrophilic modifying nanofiltration membrane；
(3) it the preparation of amphipathic modified polyamide nanofiltration membrane: in the film surface of previous step hydrophilic modifying nanofiltration membrane, pours into and matches
The ethanol solution for the perfluoro decyl trichlorosilane set, after reacting a period of time, the extra solution of removal film surface dries,
It is reacted 5-15 minutes in 60-90 DEG C of baking oven, the amphipathic modification of polyamide nanofiltration membrane is realized with this, it is poly- to obtain amphipathic modification
Amide nanofiltration membrane.
Further, the molecular cut off of ultrafiltration membrane used is 60000~100000, and preferably molecular cut off is 80000.
Further, the material of the ultrafiltration membrane is one of polysulfones, polyether sulfone, Kynoar, polypropylene.
Further, step (1) is specifically according to being implemented as follows: ultrafiltration membrane being fixed with frame, the piperazine that will be prepared first
It is poured on ultrafiltration membrane surface with the mixed aqueous solution of surfactant, mixed aqueous solution is outwelled be used in combination after a certain period of time by aqueous phase reactions
Pure water rinsing film surface, dries；The hexane solution of the pyromellitic trimethylsilyl chloride prepared is then poured over film surface, it is organic opposite
Certain time is answered, outwell solution after the completion of interface polymerization reaction and rinses film surface with n-hexane, dries, film is placed on
It is post-processed 5-20 minutes in 50-70 DEG C of baking oven, obtains initial native state nanofiltration membrane.
Further, the mixed aqueous solution of piperazine and neopelex, piperazine concentration are 0.1%~0.8wt%
(preferably 0.5wt%), surfactant concentration are 0.1~1.0wt% (preferably 0.1wt%).
Further, the concentration of the hexane solution of pyromellitic trimethylsilyl chloride is 0.05%~0.15wt% (preferably 0.09-
0.1wt%).
Further, in step (1), the aqueous phase reactions time is 30~120s (preferably 120s), and the organic phase reaction time is
30~120s (preferably 60s).
Further, in step (2), in the ethanol solution of triethanolamine, the volumetric concentration of triethanolamine be 1~5% (v:
V), preferably 4%；Reaction time is 2min~30min, preferably 2min.
Further, in step (3), in the ethanol solution of perfluoro decyl trichlorosilane, the volume of perfluoro decyl trichlorosilane
Concentration be 0.05~0.15% (v:v), preferably 0.05%；Reaction time is 2min~30min, preferably 2min.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides one kind simply, facilitates operation, at room temperature with regard to the system of reactive amphipathic antipollution nanofiltration membrane
Preparation Method is respectively first water phase, organic phase monomer using piperazine and pyromellitic trimethylsilyl chloride, and interfacial polymerization prepares polyamide and receives
Filter membrane；Then, hydrophilic triethanolamine by with remaining acyl chlorides key reactive grafting to film surface, improve the hydrophily of film；Most
Afterwards, low-surface-energy material perfluoro decyl trichlorosilane is grafted to nanofiltration film surface by closing with the hydroxyl hydrogen of triethanolamine bond,
Thus the amphipathic modified polyamide nanofiltration membrane of antifouling property raising is prepared, amphipathic modified polyamide nanofiltration membrane improves
Antifouling property of the film in multiple pollutant.
Detailed description of the invention
Fig. 1 is the amphipathic modified polyamide nanofiltration membrane preparation process schematic diagram of the present invention；
Fig. 2 is the surface electron microscope of film in embodiment 1, in which: (a) ultrafiltration membranes surface electron microscope, (b) polyamide nanofiltration
Film surface electron microscope, (c) the polyamide nanofiltration film surface electron microscope after hydrophilic modifying, (d) amphipathic modified polyamide is received
Filter membrane surface electron microscope；
Fig. 3-1,3-2,3-3 are antipollution effect figure of the different films to different pollutants of the preparation of embodiment 1, wherein PA:
Polyamide nanofiltration membrane；H-PA: the nanofiltration membrane after hydrophilic modifying；F-PA: amphipathic modified nanofiltration membrane.
Specific embodiment
Preferred embodiment of the invention is described in detail below, so that contents of the present invention feature is easy to by this field
Researcher understand, be not intended to limit the scope of the present invention.
Embodiment 1
The dodecyl sodium sulfate for weighing 1.25g piperazine and 0.25g is dissolved in water, and ultrasound is transferred to after completely dissolution
In 250mL volumetric flask, pure water constant volume.The pyromellitic trimethylsilyl chloride for weighing 0.3125g is dissolved in the n-hexane of 500mL, is put into magnetic
Son is sufficiently stirred on magnetic stirring apparatus and makes it completely dissolved.It measures 4mL triethanolamine to be dissolved in ethyl alcohol, ultrasonic dissolution is complete
It is cooled to room temperature, is then transferred into 100mL volumetric flask, ethyl alcohol constant volume after complete.The perfluoro decyl trichlorine of liquid-transfering gun measurement 0.1mL
Silane is added dropwise in the 200mL ethyl alcohol that stirred.4~6h is persistently stirred on magnetic stirring apparatus to being completely dissolved.
The preparation process figure of amphipathic modified nanofiltration membrane is as shown in Figure 1.By polysulfones ultrafiltration membranes (molecular cut off 80000)
It is fixed with the polytetrafluoroethylene (PTFE) frame of 20cm × 20cm, the piperazine aqueous solution prepared is poured on film surface first, it will after 2min
Pure water rinsing film surface is outwelled and used to aqueous phase solution, dries.The pyromellitic trimethylsilyl chloride hexane solution prepared is then poured on film
Solution is outwelled after 1min and rinses film surface with hexane solution, dried by surface.Film is placed in 60 DEG C of baking oven and is post-processed
10 minutes, obtain initial polyamide nanofiltration membrane.
Polyamide sodium filter membrane obtained continues to be modified.The triethanolamine ethanol solution prepared is poured on film table first
Face, outwells solution after 2min and respectively with ethyl alcohol, pure water rinsing film surface, dries.This is the nanofiltration membrane after hydrophilic modifying.
The perfluoro decyl trichlorosilane ethanol solution prepared is then poured on to the nanofiltration film surface after hydrophilic modifying, after 2min
Solution is outwelled and uses ethyl alcohol, pure water rinsing film surface respectively, is dried.Film is placed in 80 DEG C of baking oven and is post-processed 10 minutes,
Obtain the polyamide nanofiltration membrane of amphipathic modification.
Amphipathic Modified Membrane can obtain hydrophilic modifying film during the preparation process.In order to preferably probe into amphipathic Modified Membrane
Antifouling property, the present invention have carried out not three kinds of initial polyamide sodium filter membrane, hydrophilic modifying film and amphipathic Modified Membrane films
Antipollution with pollutant is tested, as a result as shown in Figure 3.For amphipathic Modified Membrane compared with other two film, flux rate of descent is lower,
Flux recovery rate is higher, thus antifouling effect is more preferable.
Embodiment 2
The concentration of piperazine in examples detailed above 1 is changed to 0.7wt%, other steps are constant.
Embodiment 3
The concentration of pyromellitic trimethylsilyl chloride in examples detailed above 1 is changed to 0.15wt%, other steps are constant.
Embodiment 4
The concentration of triethanolamine ethanol solution in examples detailed above 1 is changed to 5%, other steps are constant.
Embodiment 5
The concentration of perfluoro decyl trichlorosilane ethanol solution in examples detailed above 1 is changed to 0.1%, other steps are constant.
Embodiment 6
The organic phase reaction time in examples detailed above 1 is changed to 120s, other steps are constant.
Embodiment 7
The heat treatment temperature of nanofiltration membrane in an oven initial in examples detailed above 1 is changed to 100 DEG C, other steps are constant.
Embodiment 8
The heat treatment time of nanofiltration membrane film initial in examples detailed above 1 in an oven is changed to 20min, other steps are constant.
Embodiment 9
The heat treatment temperature of modified nanofiltration membrane amphipathic in examples detailed above 1 in an oven is changed to 100 DEG C, other steps are not
Become.
Embodiment 10
The heat treatment time of modified nanofiltration membrane film amphipathic in examples detailed above 1 in an oven is changed to 20min, other steps
It is constant.
Claims (10)
1. a kind of preparation method of amphipathic modified polyamide nanofiltration membrane carries out in accordance with the following steps:
(1) preparation of polyamide nanofiltration membrane: use ultrafiltration membrane as support membrane, using piperazine as aqueous phase monomers, pyromellitic trimethylsilyl chloride
For oil phase monomer, surfactant is water phase additive, and active separating layer is formed on ultrafiltration membrane using interfacial polymerization, is made
Initial polyamide nanofiltration membrane；The surfactant be dodecyl sodium sulfate, neopelex, stearic acid or
One or more of ammonium lauryl sulfate；
(2) preparation of hydrophilic modifying nanofiltration membrane: initial polyamide nanofiltration membrane is fixed with frame, is poured into and is configured on its surface
Triethanolamine ethanol solution, after reacting a period of time, the extra solution of removal film surface dries, realizes polyamide with this
The hydrophilic modifying of nanofiltration membrane obtains hydrophilic modifying nanofiltration membrane；
(3) it the preparation of amphipathic modified polyamide nanofiltration membrane: in the film surface of previous step hydrophilic modifying nanofiltration membrane, pours into and configures
Perfluoro decyl trichlorosilane ethanol solution, after reacting a period of time, the extra solution of removal film surface dries, in 60-90
DEG C baking oven in react 5-15 minutes, the amphipathic modification of polyamide nanofiltration membrane is realized with this, obtains amphipathic modified polyamide
Nanofiltration membrane.
2. preparation method as described in claim 1, it is characterised in that: the molecular cut off of ultrafiltration membrane used be 60000~
100000, preferably molecular cut off is 80000；The material of the ultrafiltration membrane is polysulfones, polyether sulfone, Kynoar, poly- third
One of alkene.
3. preparation method as claimed in claim 2, it is characterised in that: the molecular cut off of ultrafiltration membrane used is 80000.
4. the preparation method as described in one of claims 1 to 3, it is characterised in that: step (1) is specifically according to being implemented as follows: will
Ultrafiltration membrane is fixed with frame, and the mixed aqueous solution of the piperazine prepared and surfactant is poured on ultrafiltration membrane surface, water first
Pure water rinsing film surface is outwelled after a certain period of time and used to mixed aqueous solution by phase reaction, dries；The equal benzene front three that will then prepare
The hexane solution of acyl chlorides is poured over film surface, and organic phase reaction certain time falls solution after the completion of interface polymerization reaction
Fall and rinse film surface with n-hexane, dries, film is placed in 50-70 DEG C of baking oven and is post-processed 5-20 minutes, obtain initial original
Ecological nanofiltration membrane.
5. preparation method as claimed in claim 4, it is characterised in that: the mixed aqueous solution of the piperazine and surfactant,
Piperazine concentration is 0.1%~0.8wt%, and surfactant concentration is 0.1~1.0wt%；The pyromellitic trimethylsilyl chloride just oneself
The concentration of alkane solution is 0.05%~0.15wt%.
6. preparation method as claimed in claim 5, it is characterised in that: the mixed aqueous solution of the piperazine and surfactant,
Piperazine concentration is 0.5wt%, surfactant concentration 0.1wt%.
7. preparation method as claimed in claim 5, it is characterised in that: the concentration of the hexane solution of the pyromellitic trimethylsilyl chloride
For 0.09-0.1wt%.
8. preparation method as claimed in claim 4, it is characterised in that: in step (1), the aqueous phase reactions time is 30~120s
(preferably 120s), organic phase reaction time are 30~120s (preferably 60s).
9. the preparation method as described in one of claims 1 to 3, it is characterised in that: in step (2), the second of the triethanolamine
In alcoholic solution, the concentration of volume percent of triethanolamine is 1~5%, preferably 4%；Reaction time is 2min~30min, excellent
Select 2min.
10. the preparation method as described in one of claims 1 to 3, it is characterised in that: in step (3), the perfluoro decyl trichlorine
In the ethanol solution of silane, the concentration of volume percent of perfluoro decyl trichlorosilane is 0.05~0.15%, preferably 0.05%；
Reaction time is 2min~30min, preferably 2min.
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| CN109731486A (en) * | 2019-03-08 | 2019-05-10 | 浙江工业大学 | Nanofiltration membrane and preparation method thereof with brush amphoteric ion polymer decorative layer |
| CN111420561A (en) * | 2020-04-30 | 2020-07-17 | 万华化学集团股份有限公司 | Preparation method of antibacterial water-softening nanofiltration membrane and antibacterial water-softening nanofiltration membrane prepared by same |
| CN111530296A (en) * | 2020-04-29 | 2020-08-14 | 浙江工业大学 | Polyamide reverse osmosis membrane based on fluorine-containing dichlorosilane and preparation method thereof |
| CN112191114A (en) * | 2020-09-27 | 2021-01-08 | 泰州禾益新材料科技有限公司 | Polymer ultrafiltration membrane applied to polyamide composite membrane support and preparation method thereof |
| CN112387133A (en) * | 2019-08-13 | 2021-02-23 | 中国科学院大连化学物理研究所 | Preparation of polyamide composite membrane |
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| CN111530296A (en) * | 2020-04-29 | 2020-08-14 | 浙江工业大学 | Polyamide reverse osmosis membrane based on fluorine-containing dichlorosilane and preparation method thereof |
| CN111420561A (en) * | 2020-04-30 | 2020-07-17 | 万华化学集团股份有限公司 | Preparation method of antibacterial water-softening nanofiltration membrane and antibacterial water-softening nanofiltration membrane prepared by same |
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| CN112191114B (en) * | 2020-09-27 | 2021-06-18 | 泰州禾益新材料科技有限公司 | Polymer ultrafiltration membrane applied to polyamide composite membrane support and preparation method thereof |
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| CN113786738A (en) * | 2021-08-26 | 2021-12-14 | 同济大学 | Method for recycling scrapped low-pressure membrane based on interface wettability regulation and control and polyamide nanofiltration membrane prepared by method |
| CN114259884A (en) * | 2021-12-27 | 2022-04-01 | 南京理工大学 | Positively charged composite nanofiltration membrane based on in-situ zwitterionic and preparation method thereof |
| CN114749030A (en) * | 2022-03-29 | 2022-07-15 | 杭州水处理技术研究开发中心有限公司 | Nanofiltration membrane and preparation method and application thereof |
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