CN105289328B - Multiplexing type PVDF filter membranes and its preparation technology - Google Patents
Multiplexing type PVDF filter membranes and its preparation technology Download PDFInfo
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Abstract
The present invention relates to a kind of multiplexing type PVDF filter membranes, raw material includes PVDF, PEG600, PVP K30, PVP K90, water, glycerine and DMAC.The preparation method of the filter membrane is further related to, including is added raw materials into order in container successively, constant temperature stirring, spinning solution is made；Spinning solution is delivered to spinning appts, fiber is outwards extruded through spinning head, obtains just film；First film passes through phase separation groove, condensate tank(trap) and pore-forming water bath successively, obtains into pore membrane；It will be wound into pore membrane, steam shaping, film forming.The beneficial effects of the invention are as follows：Advantages of simple is formulated, reduces DMAC dosage, environmental protection；It can promote to adjust cloud point in rich or poor phase separation using the design of mixing and water adding；Preparation technology saves, and reduces water consumption during washing pore-forming, water-saving, power saving；Manufactured filter membrane is reusable, easy to operate, reduces cost；Technique and material are safe to the human body nontoxic, using trusting；Micropore precision is good to water body harmful microorganism removal effect, safe drinking water is guaranteed.
Description
Technical field
The present invention relates to a kind of multiplexing type PVDF filter membranes and its preparation technology.
Background technology
PVDF hollow fiber ultrafiltration membranes have intrinsic advantage and feature, are mainly shown as without supporter, in membrane module
Loading density is big and the membrane area of unit volume is big, also therefore more in biotechnology, gas separation, large-scale industry and medicine etc.
Field is used widely, the impurity such as colloid, suspension, bacterium and silt being commonly used in water removal.
In fact, in the milipore filter of our daily clean water treatment industries, the overwhelming majority all uses PVDF ultrafiltration membrane
Component, its filter type also tend to take grossflow filtration, periodically turn on drain valve progress pollution discharging thing or cross-flow filtration exists
Duty water opens sewage valve discharge 5-10% sewage simultaneously.
The runner of common PVDF ultrafiltration membrane causes it easily to adhere to dirt in runner according to small, can so reduce ultrafiltration
For membrane lifetime, it is necessary to carry out the dirt that regularly backwash is attached to clearly film surface with stripping to PVDF ultrafiltration membrane, the clear process of backwash is complicated,
And cleaning performance is bad；Or water body pretreatment work is carried out, filter out the inorganic matter, colloid and solid suspension of bulky grain.
In addition, in PVDF thin film preparation process, a large amount of poisonous cosolvents are commonly used, these cosolvents can remain in thin
In film, environment is polluted.Meanwhile also need to use substantial amounts of water, waste water resource during preparation.
On the basis of existing, we are improved to PVDF thin film, so provide it is a kind of may be reused it is environmentally friendly
PVDF thin film.
The content of the invention
The technical problem to be solved in the present invention is：Based on above mentioned problem, the present invention provide a kind of multiplexing type PVDF filter membranes and
Its preparation technology.
A technical scheme is used by the present invention solves its technical problem：A kind of multiplexing type PVDF filter membranes, raw material are pressed
Mass percent meter, including PVDF 20~25%, PEG600 24~34%, PVP K30 5~8%, poly- second
Alkene pyrrolidone K90 1~3%, water 5~8%, glycerine 5~10% and DMAC 30~40%.
Further, multiplexing type PVDF filter membranes, raw material by mass percentage, including PVDF 20%, PEG600
26.5%th, PVP K30 5%, PVP K90 1.5%, water 5%, glycerine 5% and DMAC
37%.
Further, multiplexing type PVDF filter membranes, raw material by mass percentage, including PVDF 22%, PEG600 25%,
PVP K30 6%, PVP K90 2%, water 6%, glycerine 6% and DMAC 33%.
Further, multiplexing type PVDF filter membranes, raw material by mass percentage, including PVDF 21%, PEG600 25%,
PVP K30 6%, PVP K90 2%, water 5%, glycerine 6% and DMAC 35%.
The preparation technology of multiplexing type PVDF filter membranes, comprises the following steps：
(1) DMAC of the glycerine of percentage by weight 5~10% and percentage by weight 30~40% is added to 50 DEG C of container
In, 90 DEG C are warming up to, constant temperature stirring；
(2) PEG600 of percentage by weight 24~34% is added in the system of step (1), 90 DEG C of constant temperature stirrings；
(3) water of percentage by weight 5~8% is added in the system of step (2), 90 DEG C of constant temperature stirrings；
(4) PVP K90 of percentage by weight 1~3% is added in the system of step (3), 90 DEG C of constant temperature
Stirring；
(5) PVP K30 of percentage by weight 5~8% is added in the system of step (4), 90 DEG C of constant temperature
Stirring；
(6) PVDF of percentage by weight 20~25% is added in the system of step (5), 90 DEG C of constant temperature stirrings, is made and spins
Silk liquid；
(7) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed through into container, spinning solution is through level
The exit orifice for three concentric diplopore spinning heads being arranged in the distribution pipe of external container sprays, and obtains just film；
(8) just film successively by 80 DEG C of phase separation grooves, 60 DEG C of condensate tank(trap)s and 30 DEG C into hole slot water-bath, obtains into pore membrane；
(9) will be wound into pore membrane, 100 DEG C of steam shaping 30min, film forming.
Further, 90 DEG C of constant temperature mixings time are at least 2h in step (1)~(6) either step, raw material with 12h
All add and finish, the duration summation of 90 DEG C of constant temperature stirrings is 48h.
Further, pumping air exhausting device, the water-bath of first film are respectively connected with above phase separation groove and condensate tank(trap) in step (8)
Speed is 20m/min, and separating tank is used to separate DMAC, and condensate tank(trap) is used to separate inorganic matter and other cosolvents, into hole slot so that
First film good moldability, pore-forming are stable.
The beneficial effects of the invention are as follows：1st, advantages of simple is formulated, reduces DMAC dosage, environmental protection；2nd, using mixing and water adding
Design can promote to adjust cloud point in rich or poor phase separation；3rd, preparation technology saves, and reduces water consumption during washing pore-forming, saves
Water, power saving；4th, manufactured filter membrane is reusable, easy to operate, reduces cost；5th, technique and material are safe to the human body nontoxic,
Using trusting；6th, micropore precision is good to water body harmful microorganism removal effect, safe drinking water is guaranteed.
Brief description of the drawings
The present invention is further described below in conjunction with the accompanying drawings.
Fig. 1 is the attenuation test curve map of multiplexing type PVDF filter membranes；
Fig. 2 is preparation technology flow chart of the present invention.
Embodiment
Presently in connection with specific embodiment, the invention will be further described, following examples be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
(1) DMAC of the glycerine of percentage by weight 5% and percentage by weight 37% is added in 50 DEG C of container, be warming up to
90 DEG C, constant temperature stirring 2h；The PEG600 of percentage by weight 26.5% is added in above-mentioned system, 90 DEG C of constant temperature stir 2h；Will weight
The water for measuring percentage 5% is added in above-mentioned system, and 90 DEG C of constant temperature stir 2h；By the polyvinylpyrrolidine of percentage by weight 1.5%
Ketone K90 is added in above-mentioned system, and 90 DEG C of constant temperature stir 2h；The PVP K30 of percentage by weight 5% is added above-mentioned
In system, 90 DEG C of constant temperature stir 2h；The PVDF of percentage by weight 20% is added in above-mentioned system, 90 DEG C of constant temperature stir 38h, system
Obtain spinning solution.
(2) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed through into container, spinning solution is through level
It is arranged in the distribution pipe of external container, distribution pipe is with 0.01~4ml/min flow from the outer of three concentric diplopore spinning heads
Hole sprays, and the pressure sensor in distribution pipe carries out flow to distribution pipe and monitored in real time, and Fluid pressure is believed
Number feed back on controller, admission pressure in controller control container, obtain just film.
(3) just film with 20m/min speed successively by 80 DEG C of phase separation grooves, 60 DEG C of condensate tank(trap)s and 30 DEG C into hole slot water
Bath, phase separation groove and condensate tank(trap) overall length 20m, pore-forming flute length are 30m, are obtained mature and stable into pore membrane.
(4) will be wound into pore membrane, 100 DEG C of steam shaping 30min, finished product.
Embodiment 2
(1) DMAC of the glycerine of percentage by weight 6% and percentage by weight 33% is added in 50 DEG C of container, be warming up to
90 DEG C, constant temperature stirring 2h；The PEG600 of percentage by weight 25% is added in above-mentioned system, 90 DEG C of constant temperature stir 3h；By weight
The water of percentage 6% is added in above-mentioned system, and 90 DEG C of constant temperature stir 2h；By the PVP K90 of percentage by weight 2%
Add in above-mentioned system, 90 DEG C of constant temperature stir 3h；The PVP K30 of percentage by weight 6% is added into above-mentioned system
In, 90 DEG C of constant temperature stir 2h；The PVDF of percentage by weight 22% is added in above-mentioned system, 90 DEG C of constant temperature stir 36h, are made and spin
Silk liquid.
(2) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed through into container, spinning solution is through level
It is arranged in the distribution pipe of external container, distribution pipe is with 0.01~4ml/min flow from the outer of three concentric diplopore spinning heads
Hole sprays, and the pressure sensor in distribution pipe carries out flow to distribution pipe and monitored in real time, and Fluid pressure is believed
Number feed back on controller, admission pressure in controller control container, obtain just film.
(3) just film with 20m/min speed successively by 80 DEG C of phase separation grooves, 60 DEG C of condensate tank(trap)s and 30 DEG C into hole slot water
Bath, phase separation groove and condensate tank(trap) overall length 20m, pore-forming flute length are 30m, are obtained mature and stable into pore membrane.
(4) will be wound into pore membrane, 100 DEG C of steam shaping 30min, finished product.
Embodiment 3
(1) DMAC of the glycerine of percentage by weight 6% and percentage by weight 35% is added in 50 DEG C of container, be warming up to
90 DEG C, constant temperature stirring 2h；The PEG600 of percentage by weight 25% is added in above-mentioned system, 90 DEG C of constant temperature stir 3h；By weight
The water of percentage 5% is added in above-mentioned system, and 90 DEG C of constant temperature stir 3h；By the PVP K90 of percentage by weight 2%
Add in above-mentioned system, 90 DEG C of constant temperature stir 2h；The PVP K30 of percentage by weight 6% is added into above-mentioned system
In, 90 DEG C of constant temperature stir 2h；The PVDF of percentage by weight 21% is added in above-mentioned system, 90 DEG C of constant temperature stir 36h, are made and spin
Silk liquid.
(2) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed through into container, spinning solution is through level
It is arranged in the distribution pipe of external container, distribution pipe is with 0.01~4ml/min flow from the outer of three concentric diplopore spinning heads
Hole sprays, and the pressure sensor in distribution pipe carries out flow to distribution pipe and monitored in real time, and Fluid pressure is believed
Number feed back on controller, admission pressure in controller control container, obtain just film.
(3) just film with 20m/min speed successively by 80 DEG C of phase separation grooves, 60 DEG C of condensate tank(trap)s and 30 DEG C into hole slot water
Bath, phase separation groove and condensate tank(trap) overall length 20m, pore-forming flute length are 30m, are obtained mature and stable into pore membrane.
(4) will be wound into pore membrane, 100 DEG C of steam shaping 30min, finished product.
The performance test results of multiplexing type PVDF filter membranes are shown in Table 1：
The performance test results of table 1, multiplexing type PVDF filter membranes
| Water flux | Durability | Toxicity | Escherichia coli clearance | |
| Embodiment 1 | 4412ml/m2, 0.1MPa, 25 DEG C | Repeatedly | It is nontoxic | >99.999% |
| Embodiment 2 | 4200ml/m2, 0.1MPa, 25 DEG C | Repeatedly | It is nontoxic | >99.999% |
| Embodiment 3 | 4000ml/m2, 0.1MPa, 25 DEG C | Repeatedly | It is nontoxic | >99.999% |
The attenuation test data of multiplexing type PVDF filter membranes are shown in Table 2 made from embodiment 1：
The attenuation test data of multiplexing type PVDF filter membranes made from table 2, embodiment 1
| Total water amount T | 0T | 1T | 2T | 3T | 4T | 5T | 6T | 7T | 8T | 9T | 10T | 11T |
| Water flux mL/min 0.1MPa | 4412 | 4306 | 4217 | 4018 | 3896 | 3653 | 3374 | 2970 | 2604 | 2203 | 1743 | 1355 |
| Total water amount T | 12T | 12T | 13T | 14T | 15T | 16T | 17T | 18T | 19T | 20T | 21T | 22T |
| Water flux mL/min 0.1MPa | 1089 | 4367 | 4210 | 4180 | 3917 | 3741 | 3508 | 3234 | 2897 | 2509 | 2054 | 1637 |
| Total water amount T | 23T | 23T | 24T | 25T | 26T | 27T | 28T | 29T | 30T | 31T | 32T | 33T |
| Water flux mL/min 0.1MPa | 1145 | 4244 | 4118 | 3875 | 3750 | 3544 | 3196 | 2810 | 2582 | 2144 | 1756 | 1211 |
| Total water amount T | 33T | 34T | 35T | 36T | 37T | 38T | 39T | 40T | 41T | 42T | 43T | 43T |
| Water flux mL/min 0.1MPa | 4135 | 3915 | 3764 | 3570 | 3262 | 2896 | 2573 | 2176 | 1848 | 1470 | 1055 | 3870 |
| Total water amount T | 44T | 45T | 46T | 47T | 48T | 49T | 50T | 51T | ||||
| Water flux mL/min 0.1MPa | 3642 | 3325 | 2907 | 2611 | 2184 | 1797 | 1354 | 1108 |
The attenuation test curve of multiplexing type PVDF filter membranes is shown in Fig. 1.From table 2 and Fig. 1, reach 12 tons in total water amount
Afterwards, water flux declines, and carries out first time washing, 4367ml/min, 0.1MPa, 25 DEG C can be reached by washing rear water flux；After water 11
After ton, water flux declines, and carries out second and washes, 4244ml/min, 0.1MPa, 25 DEG C can be reached by washing rear water flux；After water
After 10 tons, water flux declines, and carries out third time washing, 4135ml/min, 0.1MPa, 25 DEG C can be reached by washing rear water flux；After
After 10 tons of water, water flux declines, and carries out the 4th washing, 3870ml/min, 0.1MPa, 25 DEG C can be reached by washing rear water flux.By
This is visible, and water flux can maintain higher scope, and water flux and can returns to peak value after washing, reuses often, property
Can be stable.
The quality inspection of multiplexing type PVDF filter membranes
The method of inspection uses《The drinking water standard method of inspection》(GB/T5750-2006)；Sample treatment according to
《Drinking Water transmission ＆ distribution wetting system and protective materials Hygienic safety evaluation specification》(2001) appendix A is carried out.Sample soaks hydromining
Saved and prepared with appendix A 1.3.1.
As a result show：The volume of multiplexing type PVDF filter membranes is involved in drug traffic, turbidity, smelly and taste, naked eyes visible, pH, dissolubility are total
Solid, oxygen demand are (with O2Meter), arsenic, cadmium, aluminium, lead, mercury, volatile phenol, chloroform, chromium (sexavalence) index meet the Ministry of Public Health
《Drinking Water transmission ＆ distribution wetting system and protective materials Hygienic safety evaluation specification》(2001) requirement.
Escherichia coli clearance：With reference to MOH《Drinking Water water quality treater is safe and healthy with functional evaluation specification-one
As water quality treater》＆GB/T5750.12-2006 drinking water standard method of inspection microbiological indicators.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (6)
1. a kind of multiplexing type PVDF filter membranes, it is characterized in that：Raw material by mass percentage, including PVDF 20~25%, PEG600
24~34%, PVP K30 5~8%, PVP K90 1~3%, water 5~8%, glycerine 5~
10% and DMAC 30~40%；
Preparation technology comprises the following steps：
(1) DMAC of the glycerine of percentage by weight 5~10% and percentage by weight 30~40% is added in 50 DEG C of container, risen
To 90 DEG C, constant temperature stirs temperature；
(2) PEG600 of percentage by weight 24~34% is added in the system of step (1), 90 DEG C of constant temperature stirrings；
(3) water of percentage by weight 5~8% is added in the system of step (2), 90 DEG C of constant temperature stirrings；
(4) PVP K90 of percentage by weight 1~3% is added in the system of step (3), 90 DEG C of constant temperature stirrings；
(5) PVP K30 of percentage by weight 5~8% is added in the system of step (4), 90 DEG C of constant temperature stirrings；
(6) PVDF of percentage by weight 20~25% is added in the system of step (5), 90 DEG C of constant temperature stirrings, spinning solution is made；
(7) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed through into container, spinning solution is through horizontally disposed
The exit orifice of three concentric diplopore spinning heads in the distribution pipe of external container sprays, and obtains just film；
(8) just film successively by 80 DEG C of phase separation grooves, 60 DEG C of condensate tank(trap)s and 30 DEG C into hole slot water-bath, obtains into pore membrane；
(9) will be wound into pore membrane, 100 DEG C of steam shaping 30min, film forming.
2. multiplexing type PVDF filter membranes according to claim 1, it is characterized in that：Raw material by mass percentage, including PVDF
20%th, PEG600 26.5%, PVP K30 5%, PVP K90 1.5%, water 5%, glycerine
5% and DMAC 37%.
3. multiplexing type PVDF filter membranes according to claim 1, it is characterized in that：Raw material by mass percentage, including PVDF
22%th, PEG600 25%, PVP K30 6%, PVP K90 2%, water 6%, the and of glycerine 6%
DMAC 33%.
4. multiplexing type PVDF filter membranes according to claim 1, it is characterized in that：Raw material by mass percentage, including PVDF
21%th, PEG600 25%, PVP K30 6%, PVP K90 2%, water 5%, the and of glycerine 6%
DMAC 35%.
5. multiplexing type PVDF filter membranes according to claim 1, it is characterized in that：In described step (1)~(6) either step
90 DEG C of constant temperature mixings time are at least 2h, and raw material is finished in all being added in 12h, the duration summation of 90 DEG C of constant temperature stirrings
For 48h.
6. multiplexing type PVDF filter membranes according to claim 1, it is characterized in that：Phase separation groove and cold in described step (8)
Pumping air exhausting device is respectively connected with above solidifying groove, the water-bath speed of first film is 20m/min.
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