CN105709609B - A kind of preparation method of hollow fiber nanofiltration membrane - Google Patents
A kind of preparation method of hollow fiber nanofiltration membrane Download PDFInfo
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- CN105709609B CN105709609B CN201610224115.8A CN201610224115A CN105709609B CN 105709609 B CN105709609 B CN 105709609B CN 201610224115 A CN201610224115 A CN 201610224115A CN 105709609 B CN105709609 B CN 105709609B
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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
- 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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D67/0093—Chemical modification
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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
- 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
- B01D71/66—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
- 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
- B01D2323/00—Details relating to membrane preparation
- B01D2323/40—Details relating to membrane preparation in-situ membrane formation
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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
- B01D2325/24—Mechanical properties, e.g. strength
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/40—Fibre reinforced membranes
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- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of blending of whisker and polyvinyl alcohol（PVA）The method that pretreatment prepares hollow fiber nanofiltration membrane.Its main technical characteristics is：Whisker is added in polymeric casting film liquid, it is spun into hollow fiber ultrafiltration membrane, hollow fiber ultrafiltration membrane inner surface or outer surface are precoated with PVA and ionic liquid aqueous solution, then piperazine and the interfacial polymerization of pyromellitic trimethylsilyl chloride original position are carried out in pretreating surface, hollow fiber nanofiltration membrane is made.There is high mechanical strength using hollow fiber nanofiltration membrane prepared by the method；Its functional layer is more fine and close, uniform, and what is combined with basement membrane is closer, not easily to fall off；The rejection higher of hollow fiber nanofiltration membrane, service life extend.
Description
Technical field
The present invention relates to a kind of preparation method of hollow fiber nanofiltration membrane, prepared by specially whisker blending and immobilization processing
The method of hollow fiber nanofiltration membrane belongs to seperation film manufacturing field.
Background technology
Nanofiltration (NF) is that a kind of membrane separation technique between ultrafiltration, NF membrane can remove a diameter of between reverse osmosis
The particle of 1nm or so, retention relative molecular weight are 200~1000, are less than 80% to the removal efficiency of monovalent salt, are taken off to divalent salts
Except rate is higher than 90%, similar amino acid and protein is separated, realizes separation of the high score in amount and low-molecular-weight organic matter.It is hollow
The loading density of fiber nano filtering film large specific surface area, membrane module is high, and simple for process, easy cleaning, production cost is less than other types
NF membrane, and still have at low pressures compared with high desalination performance, thus be widely used in ultra-pure water preparation, food, change
The various concentrations and separation process in the fields such as work, medicine, biochemistry, environmental protection, metallurgy.Hollow fiber nanofiltration membrane is surpassed by doughnut
Filter membrane and the desalination layer of hollow fiber ultrafiltration membrane inner surface or outer surface composition, desalination layer is generally by doughnut nanofiltration
The ultra-thin compacted zone that the interfacial polymerization in situ of film inner surface or outer surface obtains.In the production process of hollow fiber nanofiltration membrane,
The hydrophily of desalination layer influences the uniformity and compactness of desalination layer, to influence salt rejection rate and the use of hollow fiber nanofiltration membrane
Service life.
Whisker is a kind of novel enhanced filler.A kind of fiber that whisker is grown into single crystal form, diameter are very small（It is micro-
Meter level）, have many advantages, such as high intensity, high-modulus and high elongation rate.The intensity of whisker is far above other chopped strands, is mainly used as
The reinforcement of composite material, for manufacturing high strength composite.
Invention content
In order to improve existing hollow fiber nanofiltration membrane desalination layer density and in uneven thickness, functional layer is easy to fall off, and machinery is strong
Relatively low, the shortcomings that morphotropism is big, easy fracture is spent, the present invention discloses a kind of whisker blending and immobilization processing prepares doughnut and receives
A kind of method of filter membrane, it is proposed that preparation process of Novel hollow fiber nano filtering film.Steps are as follows for main film：
（1）The preparation of whisker-mixed with polymers solution
Polymer, organic solvent and perforating agent are configured to polymeric casting film liquid by a certain percentage；Casting film is added in whisker
In liquid, rear standing and defoaming is stirred evenly.
（2）The preparation of hollow fiber ultrafiltration membrane
Casting solution containing whisker and core liquid are squeezed out by the nozzle of spinneret simultaneously laggard by 5cm-20cm air baths
Enter coagulating bath, 5s-30s is stopped in coagulating bath makes polymer split-phase, and film wire is removed from godet roller and is repeatedly rushed with deionized water
It washes and impregnates 48h in deionized water to get to hollow fiber ultrafiltration membrane.
（3）The pretreatment of hollow fiber ultrafiltration membrane
After hollow fiber ultrafiltration membrane is dried, contain certain density polyvinyl alcohol in its inner surface or outer surface coating
（PVA）It is dry with the aqueous solution of ionic liquid.
（4）The preparation of hollow fiber nanofiltration membrane
Piperazine aqueous solution is applied in the hollow fiber ultrafiltration membrane inner surface pre-processed or outer surface, then applies equal benzene front three
Hollow fiber nanofiltration membrane is made in the hexane solution of acyl chlorides.
PVA and ionic liquid can reduce film tension, increase piperazine aqueous solution in the adhesive force of film surface, piperazine is made to exist
Film surface distribution is more uniformly distributed.In addition, PVA contains great amount of hydroxy group, can be combined to form ionic bond with certain whiskers, ionic bond
Form the binding strength for increasing PVA and basement membrane.After PVA and ionic liquid pretreatment, hollow fiber nanofiltration membrane inner surface
Or the desalination layer of outer surface is more fine and close, uniformly, rejection also higher.
The step（1）、（2）Whisker refers in silicon carbide, ramet, silicon nitride, carbon fiber, nano-cellulose whisker
It is one or more of.
The step（1）In, the 12 wt % of a concentration of 1wt%-of whisker.
The step（3）In, a concentration of 1 wt wt of % -10 % of ionic liquid；% -10 a concentration of 1 wt of PVA
wt %。
The step（4）In, hollow fiber nanofiltration membrane desalination layer is by piperazine and pyromellitic trimethylsilyl chloride through interfacial polymerization in situ
It forms.
Compared with traditional hollow fiber nanofiltration membrane, its advantage is that：
（1）The addition of whisker enhances the mechanical strength of hollow fiber nanofiltration membrane；
（2）After PVA and the processing of ionic liquid prepreg solution, hydrophily increases for hollow fiber nanofiltration membrane inner surface or outer surface
Add, to keep the desalination layer after interfacial polymerization more fine and close, uniform, rejection higher；
（3）Hollow fiber ultrafiltration membrane inner surface or outer surface are after PVA and the processing of ionic liquid prepreg solution, in increasing
The binding strength of whisker and desalination layer in fibre ultrafiltration film, keeps functional layer not easily to fall off.
Description of the drawings
Attached drawing（Fig. 1）For the structural schematic diagram of hollow fiber nanofiltration membrane cross section of the present invention.Wherein, 1 is super for doughnut
Filter membrane cross section, 2 be desalination layer, and 3 be whisker.
Specific implementation mode
The present invention program is further elaborated with reference to embodiment.
Embodiment 1
The silicon carbide of a concentration of 1wt% is added in polymeric casting film liquid, after dissolving deaeration, the casting film containing whisker is made
Liquid；Casting solution containing whisker and core liquid are squeezed out by the nozzle of spinneret simultaneously and enter coagulating bath after 10cm air baths,
20s is stopped in coagulating bath makes polymer split-phase, and film wire deionized water is removed from godet roller and is repeatedly rinsed and in deionization
48h is impregnated in water to get to hollow fiber ultrafiltration membrane；The ionic liquid containing 5wt% is precoated in hollow fiber ultrafiltration membrane inner surface
With the aqueous solution of the PVA of 1wt%, after dry, coating piperazine aqueous solution applies the hexane solution of pyromellitic trimethylsilyl chloride again, is made
Hollow fiber nanofiltration membrane.
Embodiment 2
The silicon carbide of a concentration of 5wt% is added in polymeric casting film liquid, after dissolving deaeration, the casting film containing whisker is made
Liquid；Casting solution containing whisker and core liquid are squeezed out by the nozzle of spinneret simultaneously and enter coagulating bath after 20cm air baths,
10s is stopped in coagulating bath makes polymer split-phase, and film wire deionized water is removed from godet roller and is repeatedly rinsed and in deionization
48h is impregnated in water to get to hollow fiber ultrafiltration membrane；The ionic liquid containing 10wt% is precoated in hollow fiber ultrafiltration membrane inner surface
The aqueous solution of the PVA of body and 5wt%, after dry, coating piperazine aqueous solution applies the hexane solution of pyromellitic trimethylsilyl chloride, system again
Obtain hollow fiber nanofiltration membrane.
Embodiment 3
The silicon carbide of a concentration of 12wt% is added in polymeric casting film liquid, after dissolving deaeration, the casting film containing whisker is made
Liquid；Casting solution containing whisker and core liquid are squeezed out by the nozzle of spinneret simultaneously and enter coagulating bath after 5cm air baths,
5s is stopped in coagulating bath makes polymer split-phase, and film wire deionized water is removed from godet roller and is repeatedly rinsed and in deionized water
48h is impregnated to get to hollow fiber ultrafiltration membrane；Hollow fiber ultrafiltration membrane inner surface precoating the ionic liquid containing 5wt% and
The aqueous solution of the PVA of 10wt%, after dry, coating piperazine aqueous solution applies the hexane solution of pyromellitic trimethylsilyl chloride again, in being made
Hollow fiber NF membrane.
Control group 1
Polymeric casting film liquid and core liquid are squeezed out by the nozzle of spinneret simultaneously and enter coagulating bath after air bath, solidifying
Gu being stopped in bath makes polymer split-phase, film wire is removed from godet roller and is repeatedly rinsed with deionized water and is impregnated in deionized water
48h is to get to hollow fiber ultrafiltration membrane；Three formyl of equal benzene is applied again in hollow fiber ultrafiltration membrane inner surface coating piperazine aqueous solution
Hollow fiber nanofiltration membrane is made in the hexane solution of chlorine.
Small test membrane module is made in film wire of the same area made from Example 1-3 and control group 1, tests：（1）It surveys
Water flux is tried,（2）Magnesium sulfate and sodium chloride rejection are tested,（3）Test tensile strength.When water flux and cutoff performance are tested,
Operating pressure is 0.6Mpa, and test system temperature is 25 DEG C.Experimental result is shown in Table 1.
Water flux, rejection and the tensile strength of 1 membrane module of table
As shown in Table 1, under the same testing conditions, doughnut made from embodiment and control group in the process of the present invention
NF membrane, test water flux change rate is 20.8%, magnesium sulfate rejection rate change rate 4.7%, and sodium chloride rejection change rate is
27.3%, tensile strength change rate is 30.8%.It these results suggest that whisker blending and hollow fiber ultrafiltration membrane prepared by the present invention
Inner surface prepares complex reverse osmosis membrane through prepreg solution processing and does not carry out better than being not added with whisker and hollow fiber ultrafiltration membrane inner surface
Prepreg solution processing prepare hollow fiber nanofiltration membrane, it is alternative be not added with whisker and hollow fiber ultrafiltration membrane inner surface do not carry out it is pre-
Hollow fiber nanofiltration membrane prepared by immersion liquid processing uses.
Claims (3)
1. a kind of whisker blending and polyvinyl alcohol（PVA）The method that pretreatment prepares hollow fiber nanofiltration membrane, this method is will be brilliant
It must be added in polymeric casting film liquid, hollow fiber ultrafiltration membrane is spinned using non-solvent phase inversion, then use and contain 1wt%-
The inner surface of the aqueous solution precoating hollow-fibre membrane of PVA and 1wt% -10wt% ionic liquid of 10wt% or outer surface, finally exist
The interfacial polymerization in situ that piperazine and pyromellitic trimethylsilyl chloride are carried out by the inner surface of pretreated hollow-fibre membrane or outer surface, obtains
To hollow fiber nanofiltration membrane.
2. as described in claim 1, a kind of whisker blending and polyvinyl alcohol（PVA）Pretreatment prepares the side of hollow fiber nanofiltration membrane
Method, it is characterised in that contain whisker in basement membrane, whisker refers to silicon carbide, ramet, silicon nitride, carbon fiber, nano-cellulose crystalline substance
Must one or more of, polymer refers to one or more of polysulfones, polyether sulfone and Kynoar, whisker it is a concentration of
0.2wt%—10wt%。
3. as described in claim 1, a kind of whisker blending and polyvinyl alcohol（PVA）Pretreatment prepares the side of hollow fiber nanofiltration membrane
Method, it is characterised in that：Hollow fiber nanofiltration membrane compacted zone is by m-phenylene diamine (MPD) piperazine and pyromellitic trimethylsilyl chloride through interfacial polymerization in situ
It forms.
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| CN201610224115.8A CN105709609B (en) | 2016-04-07 | 2016-04-07 | A kind of preparation method of hollow fiber nanofiltration membrane |
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| CN201610224115.8A CN105709609B (en) | 2016-04-07 | 2016-04-07 | A kind of preparation method of hollow fiber nanofiltration membrane |
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| CN108043227B (en) * | 2017-11-22 | 2021-03-30 | 北京新源国能科技集团股份有限公司 | Preparation method of polyvinylidene fluoride nanofiltration membrane |
| CN111054214A (en) * | 2018-10-16 | 2020-04-24 | 天津天元新材料科技有限公司 | Preparation method of composite reverse osmosis membrane |
| CN110681269B (en) * | 2019-11-20 | 2022-04-22 | 宁波建嵘科技有限公司 | Two-stage coating heterogeneous synchronous composite film preparation device |
| CN115193269A (en) * | 2021-04-14 | 2022-10-18 | 西陇科学股份有限公司 | Preparation method of high-flux fine hollow fiber nanofiltration membrane for purifying drinking water |
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| CN101524626A (en) * | 2008-03-07 | 2009-09-09 | 浙江欧美环境工程有限公司 | External pressure type hollow fiber nano filtering film and preparation method thereof |
| CN103240008A (en) * | 2012-02-08 | 2013-08-14 | 沃盛环保科技（上海）有限公司 | Whisker reinforced polyvinylidene fluoride hollow fiber film and preparation technology thereof |
| CN103041713B (en) * | 2013-01-28 | 2016-08-10 | 天津膜天膜科技股份有限公司 | A kind of preparation method of hollow fiber nanofiltration membrane |
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