CN110479117A - A kind of preparation method of the big flux hollow fibre ultrafiltration membrane of hydrophily - Google Patents
A kind of preparation method of the big flux hollow fibre ultrafiltration membrane of hydrophily Download PDFInfo
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- CN110479117A CN110479117A CN201910704236.6A CN201910704236A CN110479117A CN 110479117 A CN110479117 A CN 110479117A CN 201910704236 A CN201910704236 A CN 201910704236A CN 110479117 A CN110479117 A CN 110479117A
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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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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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
- 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
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention provides a kind of preparation method of big flux hollow fibre ultrafiltration membrane of hydrophily, comprising the following steps: (1) preparation steps of casting film feed liquid: heating stirring in feed liquid stirred autoclave is added in solvent, resin, film for additive, dispersing agent and is dissolved；(2) preparation steps of core liquid: pure water, solvent are proportionally added into core liquid reaction kettle, stirred evenly；(3) forming step of film wire: being transferred to deaeration reaction kettle for above-mentioned casting film feed liquid, remove the bubble in casting film feed liquid, is pumped into spinneret by feed liquid and realizes film wire molding；(4) solidification of film wire and cleaning step: feed liquid enters coagulating tank after spinneret, and the film wire after split-phase solidification is wrapped on wire drawing wheel by cleaning bath；(5) soaking step of film wire: film wire enters soaking compartment；Film wire after impregnating obtains finished product film wire again successively through the second soaking compartment and third rinse bath.The film wire hydrophily of preparation of the invention is strong, and flux is big, containing the elastomeric material for not working, not hydrolyzing, never degenerating with many chemicals on the substance for the blending added in formula, increases the stability and stain resistance of ultrafiltration membrane.
Description
Technical field
The present invention relates to a kind of preparation methods of the big flux hollow fibre ultrafiltration membrane of hydrophily, belong to technical field of membrane.
Background technique
Ultrafiltration membrane as a kind of membrane separation technique, be widely used in pure water produce, tap water purifying, sea water desalination,
The water treatment fields such as bitter processing, sewage treatment.Ultrafiltration membrane due to membrane material, the difference of film production process, flux,
Hydrophily, stain resistance, resistance to acid and alkali be not also identical, and the ultrafiltration membrane of traditional polysulfones, polyether sulfone material, durability against pollution is poor,
Polyvinylidene fluoride (PVDF) ultrafiltration membrane in the present invention has many advantages, such as anti-pollution, and chemical stability is high, is presently preferred ultrafiltration membrane product
One of kind.
Summary of the invention
The technical problems to be solved by the present invention are: the present invention provides a kind of preparation of ultrafiltration membrane that big flux hydrophily is strong
Method, making every effort to be made has permanent hydrophilic, chemical-resistant resistance and pollution, is not easy dirt and blocks up, and operating pressure is low, and membrane flux is big,
Filtering accuracy is high, the hollow fiber ultrafiltration membrane of separative efficiency height and easy cleaning.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The preparation method of the big flux hollow fibre ultrafiltration membrane of hydrophily provided by the invention, characterized in that it comprises the following steps:
(1) preparation steps of casting film feed liquid: solvent, resin, film for additive, dispersing agent are added in feed liquid stirred autoclave,
Heating stirring is dissolved to uniform solution；Each component parts by weight are as follows: resin: 15~25 parts；50~80 parts of solvent；Film forming addition
Agent: 10~30 parts；Dispersing agent: 6-15 parts.
(2) preparation steps of core liquid: pure water, solvent being proportionally added into core liquid reaction kettle, stirred evenly, and core liquid is by weight
The proportion measured than pure water 80, solvent 20 prepares core liquid in core liquid reaction kettle.
(3) forming step of film wire: above-mentioned casting film feed liquid is transferred to deaeration reaction kettle, sloughs the gas in casting film feed liquid
Bubble, passes through gear pump for casting film feed liquid, core liquid respectively and is input to spinneret, realizes film wire molding by spinneret；
(4): the solidification of film wire and cleaning step: the film wire of forming enters the solidification of coagulating tank split-phase, wherein spinneret is set to
There is a distance in the top of coagulating tank therewith, so that casting film feed liquid after molding can pass through one section of sky before entering coagulating tank
Gas section；The non-solvent for having certain temperature difference with casting film feed liquid is filled in coagulating tank, non-solvent can be water or water and other liquid
Mixing, also may include the mixed liquor of water and solvent.
Usually selection aqueous solution non-solvent is mainly made of water in practice, related with specific ultrafiltration membrane preparation method, at
The good feed liquid of type is in coagulating tank, and the solvent formed in feed liquid is diffused exchange in pure water, and feed liquid is frozen into film wire；At
Film wire after type solidification by cleaning bath, cleaned, solvent remaining in film wire cleaned up with additive, film by film wire
Silk is wound on wire drawing wheel.
(5) film wire soaking step: film wire is wound into a fixing turn on wire drawing wheel and cuts off, and ties up bunchy with nylon wire and moves on to
First soaking compartment, pays attention to elasticity when tying up, film wire cannot be made to be squeezed and deformed, pure water is filled in soaking compartment, makes molten in film wire
Agent is further dissolved in water, and the one-tenth porosity of film wire is increased；Film wire moves into the second soaking compartment after the first soaking compartment impregnates 48h, the
Two soaking compartments fill pure water and glycerine, and weight ratio is 90 parts of pure water, 10 parts of glycerine；Glycerine has cured film wire hole and improvement
The hydrophilic effect of film wire；Film wire the second soaking compartment impregnate 48h after move into third soaking compartment, third soaking compartment fill pure water and
With the glycerine of the second soaking compartment different proportion, weight ratio is 80 parts of pure water, 20 parts of glycerine, impregnates 48h, cleans net film wire table
The solvent in face moves back out film wire；
(6) dehydration of film wire: film wire is impregnated after a certain period of time in third soaking compartment, removes film wire, one of film wire is tied up
It pricks, is suspended on film wire hanging frame and dries dehydration (being assisted when necessary with fan and air-conditioning), dewatered film wire is infused after being packed into putamina
Glue just forms hyperfiltration membrane assembly.
Resin as matrix is polyvinylidene fluoride resin (PVDF)；Film for additive is polyvinylpyrrolidone (PVP
K30)；Solvent is dimethyl acetamide (DMAC) or dimethylformamide (DMF)；Dispersing agent is polyethylene glycol (PEG400) and tween
80(TW80).
Beneficial effects of the present invention:
Preparation method of the invention prepares hollow-fibre membrane by phase inversion, and contains on the substance for the blending added in being formulated
Some hydrophilic radicals, so that film wire has permanent hydrophilicity；Contain excellent table on the substance for the blending added in formula
Face activity and film forming characteristics group, the one-tenth porosity and hole for increasing film wire are evenly distributed with rate, increase the water flux of ultrafiltration membrane；Add in formula
Containing the elastomeric material for not working, not hydrolyzing, never degenerating with many chemicals on the substance of the blending added, ultrafiltration membrane is increased
Stability and stain resistance.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the preparation process of the big strong ultrafiltration membrane of flux hydrophily of the present invention.
In figure: 1, feed liquid stirred autoclave；2, deaeration reaction kettle；3, core liquid reaction kettle；4, feed liquid gear pump；5, core liquid
Gear pump；6, spinneret；7, coagulating tank；8, bath is cleaned；9, wire drawing wheel；10, soaking compartment；11, film wire hanging
Frame.
Specific embodiment
Embodiment 1
The present embodiment provides a kind of preparation methods of the big flux hollow fibre ultrafiltration membrane of hydrophily, including the following steps:
(1) preparation steps of casting film feed liquid: resin, solvent, film for additive and dispersing agent are added in stirred autoclave, added
Thermal agitation is dissolved to uniform solution；
Wherein: each component parts by weight are as follows: resin: 15~25 parts；50~80 parts of solvent；Film for additive: 10~30 parts；Dispersion
Agent: 6-15 parts；
Resin as matrix is polyvinylidene fluoride resin (PVDF)；Film for additive is polyvinylpyrrolidone (PVP
K30)；Solvent is dimethyl acetamide (DMAC) or dimethylformamide (DMF)；Dispersing agent is polyethylene glycol (PEG400) and tween
80(TW80).
(2) preparation steps of core liquid: pure water, solvent being proportionally added into core liquid reaction kettle, stirred evenly, and core liquid is by weight
The proportion measured than pure water 80, solvent 20 prepares core liquid in core liquid reaction kettle.
(3) forming step of film wire: the casting film feed liquid in (1) is transferred to deaeration reaction kettle, is sloughed in casting film feed liquid
Casting film feed liquid, core liquid are passed through gear pump respectively and are delivered to spinneret by bubble, realize film wire molding by spinneret.
(4) solidification of film wire and cleaning step: the film wire of forming enters the solidification of coagulating tank split-phase, wherein spinneret
There is a distance in top set on coagulating tank therewith, so that casting film feed liquid after molding can pass through one before entering coagulating tank
Section air section；The non-solvent for having certain temperature difference with casting film feed liquid is filled in coagulating tank, non-solvent can be water or water and other
The mixing of liquid also may include the mixed liquor of water and solvent.Usually selection aqueous solution non-solvent is mainly made of water in practice,
Related with specific ultrafiltration membrane preparation method, the feed liquid of forming forms the solvent in feed liquid in pure water in coagulating tank
It is diffused exchange, feed liquid is frozen into film wire；Film wire after molding solidification is by cleaning bath, and film wire is cleaned, by film wire
In remaining solvent cleaned up with additive, film wire is wound on wire drawing wheel.
(5) film wire soaking step: film wire is wound into a fixing turn on wire drawing wheel and cuts off, and ties up bunchy with nylon wire and moves on to
First soaking compartment, pays attention to elasticity when tying up, film wire cannot be made to be squeezed and deformed, pure water is filled in soaking compartment, makes molten in film wire
Agent is further dissolved in water, and the one-tenth porosity of film wire is increased；Film wire is impregnated in the first soaking compartment moves into the second immersion after a certain period of time
Slot, the second soaking compartment fill pure water and a certain proportion of glycerine, and glycerine has cured film wire hole and improvement film wire hydrophilic
Effect；Film wire is impregnated in the second soaking compartment moves into third soaking compartment after a certain period of time, and third soaking compartment fills pure water and with second
The glycerine of soaking compartment different proportion, impregnates certain time, and the solvent for cleaning net film wire surface moves back out film wire.
Firstly, preparing casting film feed liquid according to component in table 1 and its weight proportion:
The component and its proportion of 1 casting film feed liquid of table
| Serial number | Material | Parts by weight |
| 1 | PVDF Solef6010/1001 | 25 |
| 2 | DMAC | 65 |
| 3 | PVP-K30 | 15 |
| 4 | Polyethylene glycol PEG400 | 10 |
| 5 | Tween 80 | 5 |
With further reference to Fig. 1, (whipping temp is 75 DEG C, when stirring after the completion of casting film feed liquid stirs in feed liquid stirred autoclave 1
Between for for 24 hours) be transferred to deaeration spinning kettle 2, deaeration is for 24 hours under conditions of negative pressure 0.1MPa；Core liquid by weight 80 parts of pure water,
DMAC20 parts of proportion prepares core liquid in core liquid reaction kettle 3, and core liquid temperature setting is 65 DEG C；Later in the item of positive pressure 0.2MPa
Feed liquid is passed sequentially through into filter, the feeding spinneret 6 of feed liquid gear pump 4 by pipeline under part, meanwhile, in the item of positive pressure 0.2MPa
Core liquid is passed sequentially through into filter by pipeline under part, core liquid gear pump 5 is sent into spinneret 6；Pass through feed liquid gear pump 4, core liquid
The control of gear pump 5 passes through the reduction of feed volume of spinneret 6, according to the size of reduction of feed volume and spinneret film wire is formed, control is spun
Film wire internal-and external diameter is the hollow-fibre membrane of 0.7/1.3mm；Coagulating tank 7 is sequentially entered after film wire molding carries out split-phase, cleaning
Bath 8 is wound on wire drawing wheel after cleaning, to be wound that film wire is quickly cut off bunchy to after certain circle number, and at once at
The film wire of beam is wrapped with nylon wire moves on to soaking compartment 10, and soaking compartment 10 divides for 3 slots, not connected and leaching independently
Slot is steeped, wherein being put into a certain amount of pure water in the 1st soaking compartment, water, which is subject to, submerged film wire, impregnated in the 1st soaking compartment
48h further removes the solvent in film wire, increases the one-tenth porosity of film wire；Then film wire is moved into the 2nd soaking compartment, the 2nd impregnates
By weight being added 90 parts of pure water in slot, 10 parts of glycerine, soaking time 48h, glycerine can make film wire hole solidify, and guarantee
Film wire pore-forming is uniform, and keeping film wire nominal pore size is 0.03 μm；Film wire is then moved into the 3rd soaking compartment again, is pressed in the 3rd soaking compartment
Weight ratio is added 80 parts of pure water, and 20 parts of glycerine, soaking time 48h, further cured film wire hole guarantees that film wire hole forming is complete
Whole, one-tenth porosity is high, and increases the hydrophilicity of film；After film wire is impregnated, a binding of film wire, it is suspended on film frame and dries
Dehydration, injecting glue just forms hyperfiltration membrane assembly after dewatered film wire is packed into putamina.
The experimental data of the invention of embodiment 2:
After tested, the performance through the strong ultrafiltration membrane of big flux hydrophily made from this method is as follows: film wire flux is 260L/ ㎡ .H
(test pressure: 0.2MPa), produces water turbidity≤0.1NTU, film wire intensity >=4MPa, film wire one-tenth porosity >=86%.
The figures above and explanation are to be used to provide further understanding of the present invention.Obviously, the foregoing is merely the present invention
Preferable specific embodiment, but scope of protection of the present invention is not limited thereto, it is any to one skilled in the art
Be can readily occur in, essentially without change or replacement of the invention are detached from, be also all included in the scope of protection of the present invention.
Claims (3)
1. the preparation method of the big flux hollow fibre ultrafiltration membrane of hydrophily, characterized in that it comprises the following steps:
(1) preparation steps of casting film feed liquid: solvent, resin, film for additive, dispersing agent are added in feed liquid stirred autoclave,
Heating stirring is dissolved to uniform solution；Each component parts by weight are as follows: resin: 15~25 parts；50~80 parts of solvent；Film forming addition
Agent: 10~30 parts；Dispersing agent: 6-15 parts；
(2) preparation steps of core liquid: pure water, solvent are proportionally added into core liquid reaction kettle, stirred evenly；Core liquid is by weight
Pure water 80, solvent 20 proportion prepare core liquid in core liquid reaction kettle；
(3) forming step of film wire: being transferred to deaeration reaction kettle for above-mentioned casting film feed liquid, slough the bubble in casting film feed liquid, will
Casting film feed liquid, core liquid pass through gear pump respectively and are input to spinneret, realize film wire molding by spinneret；
(4): the solidification of film wire and cleaning step: the film wire of forming enters the solidification of coagulating tank split-phase, wherein spinneret is set to
There is a distance in the top of coagulating tank therewith, so that casting film feed liquid after molding can pass through one section of sky before entering coagulating tank
Gas section；The non-solvent for having certain temperature difference with casting film feed liquid is filled in coagulating tank, non-solvent can be water or water and other liquid
Mixing, also may include the mixed liquor of water and solvent.
2.(5) film wire soaking step: film wire is wound into a fixing turn on wire drawing wheel and cuts off, and ties up bunchy with nylon wire and moves on to
One soaking compartment, pays attention to elasticity when tying up, film wire cannot be made to be squeezed and deformed, pure water is filled in soaking compartment, makes the solvent in film wire
It further dissolves in water, increases the one-tenth porosity of film wire；Film wire moves into the second soaking compartment after the first soaking compartment impregnates 48h, and second
Soaking compartment fills pure water and glycerine, and weight ratio is 90 parts of pure water, 10 parts of glycerine；Glycerine has cured film wire hole and improves film
The hydrophilic effect of silk；Film wire the second soaking compartment impregnate 48h after move into third soaking compartment, third soaking compartment fill pure water and with
The glycerine of second soaking compartment different proportion, weight ratio are 80 parts of pure water, 20 parts of glycerine, impregnate 48h, clean net film wire surface
Solvent move back out film wire；
(6) dehydration of film wire: film wire is impregnated after a certain period of time in third soaking compartment, removes film wire, one of film wire is tied up
It pricks, is suspended on film wire hanging frame and dries dehydration (being assisted when necessary with fan and air-conditioning), dewatered film wire is infused after being packed into putamina
Glue just forms hyperfiltration membrane assembly.
3. the preparation method of the big flux hollow fibre ultrafiltration membrane of hydrophily according to claim 1, which is characterized in that as
The resin of matrix is polyvinylidene fluoride resin (PVDF)；Film for additive is polyvinylpyrrolidone (PVP K30)；Solvent is two
Methylacetamide (DMAC) or dimethylformamide (DMF)；Dispersing agent is polyethylene glycol (PEG400) and Tween 80 (TW80).
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Cited By (4)
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| CN111921384A (en) * | 2020-08-11 | 2020-11-13 | 浙江易膜新材料科技有限公司 | Casting membrane liquid of PVDF hollow fiber ultrafiltration membrane, spinning mechanism and production method thereof |
| CN113398772A (en) * | 2021-07-23 | 2021-09-17 | 山东招金膜天股份有限公司 | Continuous automatic soaking treatment device and method for hollow fiber membrane bundle |
| CN113856475A (en) * | 2021-10-22 | 2021-12-31 | 滁州久盈膜科技有限公司 | Rinsing method and device for hollow fiber membrane |
| CN114887496A (en) * | 2022-05-05 | 2022-08-12 | 奥赛科膜科技(天津)有限公司 | Continuous sheet-shaped hollow fiber membrane production line and process method |
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| CN114887496A (en) * | 2022-05-05 | 2022-08-12 | 奥赛科膜科技(天津)有限公司 | Continuous sheet-shaped hollow fiber membrane production line and process method |
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