CN105289328A - Reuse type PVDF filter membrane and preparation technology thereof - Google Patents
Reuse type PVDF filter membrane and preparation technology thereof Download PDFInfo
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Abstract
The invention relates to a reuse type PVDF membrane. Raw materials comprise PVDF, PEG600, polyvinylpyrrolidone K30, polyvinylpyrrolidone K90, water, glycerin and DMAC. The invention further relates to a preparation method of the filter membrane. The method includes the steps that the raw materials are added in a container in sequence and stirred at a constant temperature, and spinning liquid is prepared; the spinning liquid is conveyed to a spinning device, fibers are extruded outwards through a spinning nozzle, and a preliminary membrane is obtained; the preliminary membrane sequentially passes a phase separating tank, a condensing tank and a hole forming water bath tank, and a hole forming membrane is obtained; the hole forming membrane is wound and sized through steam, and the finished membrane is obtained. The reuse type PVDF membrane has the advantages that the formula is simple and reasonable, the use amount of DMAC is reduced, and environmental friendliness is achieved; mixed water adding design is adopted, and it is promoted that a turbidity point is adjusted in the poor and rich phase separation process; the preparation technology saves energy, the amount of water used in the water washing hole forming process is reduced, and water and electricity are saved; the prepared filter membrane can be reused, operation is convenient, and cost is reduced; the technology and materials are safe and harmless to human bodies, and a user is at ease when the filter membrane is used; the removing effect of harmful microorganisms in water is good due to micro-hole precision, and safety of drinking water is guaranteed.
Description
Technical field
The present invention relates to a kind of multiplexing type PVDF filter membrane and preparation technology thereof.
Background technology
PVDF hollow fiber ultrafiltration membrane has intrinsic advantage and feature, main manifestations is without the need to supporter, loading density in membrane module membrane area that is large and unit volume is large, also be therefore used widely biotechnology, gas separaion, large-scale industry and medicine etc. are multi-field, be commonly used to the impurity such as the colloid removed in water, suspension, bacterium and silt.
In fact, in the milipore filter of our daily clean water treatment industry, the overwhelming majority has all adopted PVDF ultrafiltration membrane assembly, its filter type also tends to take grossflow filtration, and regular unlatching drain valve carries out pollution discharging thing or cross-flow filtration opens the sewage of sewage valve discharge 5-10% at duty water simultaneously.
The runner of common PVDF ultrafiltration membrane is contrasted little and causes it easily to adhere to dirt in runner, the milipore filter life-span can be reduced like this, need to carry out regular backwash clearly to peel off the dirt being attached to face to PVDF ultrafiltration membrane, the clear process of backwash is complicated, and cleaning performance is not good; Or carry out water body pretreatment work, filter out oarse-grained inorganic matter, colloid and solid suspension.
In addition, in PVDF thin film preparation process, commonly use cosolvent poisonous in a large number, these cosolvents can remain in the film, contaminated environment.Meanwhile, also need during preparation to use a large amount of water, waste water resource.
On existing basis, we improve PVDF thin film, so provide a kind of can the PVDF thin film of reusable environmental protection.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides a kind of multiplexing type PVDF filter membrane and preparation technology thereof.
The present invention solves the technical scheme that its technical problem adopts: a kind of multiplexing type PVDF filter membrane, raw material by mass percentage, comprises PVDF20 ~ 25%, PEG60024 ~ 34%, PVP K30 5 ~ 8%, PVP K90 1 ~ 3%, water 5 ~ 8%, glycerine 5 ~ 10% and DMAC30 ~ 40%.
Further, multiplexing type PVDF filter membrane, raw material by mass percentage, comprises PVDF20%, PEG60026.5%, PVP K30 5%, PVP K90 1.5%, water 5%, glycerine 5% and DMAC37%.
Further, multiplexing type PVDF filter membrane, raw material by mass percentage, comprises PVDF22%, PEG60025%, PVP K30 6%, PVP K90 2%, water 6%, glycerine 6% and DMAC33%.
Further, multiplexing type PVDF filter membrane, raw material by mass percentage, comprises PVDF21%, PEG60025%, PVP K30 6%, PVP K90 2%, water 5%, glycerine 6% and DMAC35%.
The preparation technology of multiplexing type PVDF filter membrane, comprises the following steps:
(1) added in the container of 50 DEG C by the DMAC of the glycerine of percentage by weight 5 ~ 10% and percentage by weight 30 ~ 40%, be warming up to 90 DEG C, constant temperature stirs;
(2) added by the PEG600 of percentage by weight 24 ~ 34% in the system of step (1), 90 DEG C of constant temperature stir;
(3) added by the water of percentage by weight 5 ~ 8% in the system of step (2), 90 DEG C of constant temperature stir;
(4) added by the PVP K90 of percentage by weight 1 ~ 3% in the system of step (3), 90 DEG C of constant temperature stir;
(5) added by the PVP K30 of percentage by weight 5 ~ 8% in the system of step (4), 90 DEG C of constant temperature stir;
(6) added by the PVDF of percentage by weight 20 ~ 25% in the system of step (5), 90 DEG C of constant temperature stir, obtained spinning solution;
(7) delivered to by spinning solution in the closed container of shaping spinning appts, in container, pass into gas, the exit orifice ejection of three on the distributing pipe of spinning solution through being horizontally set on external container concentric diplopore spinning heads, obtains just film;
(8) just film becomes hole slot water-bath through 80 DEG C of grooves that are separated, 60 DEG C of condensate tank(trap)s with 30 DEG C successively, obtains into pore membrane;
(9) pore membrane rolling will be become, 100 DEG C of steam shaping 30min, film forming.
Further, in step (1) ~ (6) arbitrary step, 90 DEG C of constant temperature mixings time are at least 2h, all add complete in raw material and 12h, and the duration summation that 90 DEG C of constant temperature stirs is 48h.
Further, be all connected with bleed air exhausting device above be separated groove and condensate tank(trap) in step (8), the water-bath speed of first film is 20m/min, separating tank is for separating of DMAC, condensate tank(trap) is for separating of inorganic matter and other cosolvents, and become hole slot to make just film good moldability, pore-forming is stablized.
The invention has the beneficial effects as follows: advantages of simple of 1, filling a prescription, reduce the consumption of DMAC, environmental protection; 2, adopt the design of mixing and water adding can impel in rich or poor phase separation and regulate cloud point; 3, preparation technology is energy-conservation, reduces water consumption during washing pore-forming, water-saving, power saving; 4, the filter membrane made is reusable, easy to operate, reduces cost; 5, technique and material nontoxic to human-body safety, use relieved; 6, micropore precision is good to water body harmful microorganism removal effect, and safe drinking water is guaranteed.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described.
Fig. 1 is the attenuation test curve map of multiplexing type PVDF filter membrane;
Fig. 2 is preparation technology's flow chart of the present invention.
Detailed description of the invention
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
(1) added in the container of 50 DEG C by the DMAC of the glycerine of percentage by weight 5% and percentage by weight 37%, be warming up to 90 DEG C, constant temperature stirs 2h; Added by the PEG600 of percentage by weight 26.5% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the water of percentage by weight 5% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVP K90 of percentage by weight 1.5% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVP K30 of percentage by weight 5% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVDF of percentage by weight 20% in above-mentioned system, 90 DEG C of constant temperature stir 38h, obtained spinning solution.
(2) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed in container, on the distributing pipe of spinning solution through being horizontally set on external container, distributing pipe sprays with the exit orifice of the flow of 0.01 ~ 4ml/min from three concentric diplopore spinning heads, the pressure sensor be arranged on distributing pipe carries out flow to distributing pipe and carries out Real-Time Monitoring, and fluid pressure signal is fed back on controller, controller controls admission pressure in container, obtains just film.
(3) just film becomes hole slot water-bath through 80 DEG C of grooves that are separated, 60 DEG C of condensate tank(trap)s with 30 DEG C successively with the speed of 20m/min, and be separated groove and condensate tank(trap) overall length 20m, and pore-forming flute length is 30m, obtains mature and stable one-tenth pore membrane.
(4) pore membrane rolling will be become, 100 DEG C of steam shaping 30min, obtained finished product.
Embodiment 2
(1) added in the container of 50 DEG C by the DMAC of the glycerine of percentage by weight 6% and percentage by weight 33%, be warming up to 90 DEG C, constant temperature stirs 2h; Added by the PEG600 of percentage by weight 25% in above-mentioned system, 90 DEG C of constant temperature stir 3h; Added by the water of percentage by weight 6% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVP K90 of percentage by weight 2% in above-mentioned system, 90 DEG C of constant temperature stir 3h; Added by the PVP K30 of percentage by weight 6% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVDF of percentage by weight 22% in above-mentioned system, 90 DEG C of constant temperature stir 36h, obtained spinning solution.
(2) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed in container, on the distributing pipe of spinning solution through being horizontally set on external container, distributing pipe sprays with the exit orifice of the flow of 0.01 ~ 4ml/min from three concentric diplopore spinning heads, the pressure sensor be arranged on distributing pipe carries out flow to distributing pipe and carries out Real-Time Monitoring, and fluid pressure signal is fed back on controller, controller controls admission pressure in container, obtains just film.
(3) just film becomes hole slot water-bath through 80 DEG C of grooves that are separated, 60 DEG C of condensate tank(trap)s with 30 DEG C successively with the speed of 20m/min, and be separated groove and condensate tank(trap) overall length 20m, and pore-forming flute length is 30m, obtains mature and stable one-tenth pore membrane.
(4) pore membrane rolling will be become, 100 DEG C of steam shaping 30min, obtained finished product.
Embodiment 3
(1) added in the container of 50 DEG C by the DMAC of the glycerine of percentage by weight 6% and percentage by weight 35%, be warming up to 90 DEG C, constant temperature stirs 2h; Added by the PEG600 of percentage by weight 25% in above-mentioned system, 90 DEG C of constant temperature stir 3h; Added by the water of percentage by weight 5% in above-mentioned system, 90 DEG C of constant temperature stir 3h; Added by the PVP K90 of percentage by weight 2% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVP K30 of percentage by weight 6% in above-mentioned system, 90 DEG C of constant temperature stir 2h; Added by the PVDF of percentage by weight 21% in above-mentioned system, 90 DEG C of constant temperature stir 36h, obtained spinning solution.
(2) spinning solution is delivered in the closed container of shaping spinning appts, gas is passed in container, on the distributing pipe of spinning solution through being horizontally set on external container, distributing pipe sprays with the exit orifice of the flow of 0.01 ~ 4ml/min from three concentric diplopore spinning heads, the pressure sensor be arranged on distributing pipe carries out flow to distributing pipe and carries out Real-Time Monitoring, and fluid pressure signal is fed back on controller, controller controls admission pressure in container, obtains just film.
(3) just film becomes hole slot water-bath through 80 DEG C of grooves that are separated, 60 DEG C of condensate tank(trap)s with 30 DEG C successively with the speed of 20m/min, and be separated groove and condensate tank(trap) overall length 20m, and pore-forming flute length is 30m, obtains mature and stable one-tenth pore membrane.
(4) pore membrane rolling will be become, 100 DEG C of steam shaping 30min, obtained finished product.
The performance test results of multiplexing type PVDF filter membrane is in table 1:
The performance test results of table 1, multiplexing type PVDF filter membrane
| Water flux | Durability | Toxicity | Escherichia coli clearance | |
| Embodiment 1 | 4412ml/m 2，0.1MPa，25℃ | Repeatedly | Nontoxic | >99.999％ |
| Embodiment 2 | 4200ml/m 2，0.1MPa，25℃ | Repeatedly | Nontoxic | >99.999％ |
| Embodiment 3 | 4000ml/m 2，0.1MPa，25℃ | Repeatedly | Nontoxic | >99.999％ |
The attenuation test data of the multiplexing type PVDF filter membrane that embodiment 1 is obtained are in table 2:
The attenuation test data of the multiplexing type PVDF filter membrane that table 2, embodiment 1 are obtained
| 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 membrane is shown in Fig. 1.From table 2 and Fig. 1, after total water amount reaches 12 tons, water flux declines, and carries out first time washing, washes rear water flux and can reach 4367ml/min, 0.1MPa, 25 DEG C; After 11 tons, water, water flux declines, and carries out second time washing, washes rear water flux and can reach 4244ml/min, 0.1MPa, 25 DEG C; After 10 tons, water, water flux declines, and carries out third time washing, washes rear water flux and can reach 4135ml/min, 0.1MPa, 25 DEG C; After 10 tons, water, water flux declines, and carries out the 4th washing, washes rear water flux and can reach 3870ml/min, 0.1MPa, 25 DEG C.As can be seen here, water flux can maintain higher scope, and after washing, water flux can get back to peak value again, reuses often, stable performance.
The quality inspection of multiplexing type PVDF filter membrane
The method of inspection adopts " the drinking water standard method of inspection " (GB/T5750-2006); Sample treatment carries out according to " Drinking Water transmission & distribution wetting system and protective materials Hygienic safety evaluation specification " (2001) appendix A.Sample soaks hydromining appendix A 1.3.1 and saves preparation.
Result shows: the volume of multiplexing type PVDF filter membrane is involved in drug traffic, turbidity, smelly and taste, naked eyes visible, pH, total dissolved solid, oxygen demand be (with O
2meter), arsenic, cadmium, aluminium, lead, mercury, volatile phenol, chloroform, chromium (sexavalence) index all meet the requirement of the Ministry of Public Health " Drinking Water transmission & distribution wetting system and protective materials Hygienic safety evaluation specification " (2001).
Escherichia coli clearance: with reference to MOH " Drinking Water water quality treater safe and sanitary and functional evaluation specification-general water quality treater " & GB/T5750.12-2006 drinking water standard method of inspection microbiological indicator.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on description, must determine its technical scope according to right.
Claims (7)
1. a multiplexing type PVDF filter membrane, it is characterized in that: raw material by mass percentage, comprises PVDF20 ~ 25%, PEG60024 ~ 34%, PVP K30 5 ~ 8%, PVP K90 1 ~ 3%, water 5 ~ 8%, glycerine 5 ~ 10% and DMAC30 ~ 40%.
2. multiplexing type PVDF filter membrane according to claim 1, it is characterized in that: raw material by mass percentage, comprises PVDF20%, PEG60026.5%, PVP K30 5%, PVP K90 1.5%, water 5%, glycerine 5% and DMAC37%.
3. multiplexing type PVDF filter membrane according to claim 1, it is characterized in that: raw material by mass percentage, comprises PVDF22%, PEG60025%, PVP K30 6%, PVP K90 2%, water 6%, glycerine 6% and DMAC33%.
4. multiplexing type PVDF filter membrane according to claim 1, it is characterized in that: raw material by mass percentage, comprises PVDF21%, PEG60025%, PVP K30 6%, PVP K90 2%, water 5%, glycerine 6% and DMAC35%.
5. the preparation technology of the multiplexing type PVDF filter membrane according to any one of Claims 1 to 4, is characterized in that: comprise the following steps:
(1) added in the container of 50 DEG C by the DMAC of the glycerine of percentage by weight 5 ~ 10% and percentage by weight 30 ~ 40%, be warming up to 90 DEG C, constant temperature stirs;
(2) added by the PEG600 of percentage by weight 24 ~ 34% in the system of step (1), 90 DEG C of constant temperature stir;
(3) added by the water of percentage by weight 5 ~ 8% in the system of step (2), 90 DEG C of constant temperature stir;
(4) added by the PVP K90 of percentage by weight 1 ~ 3% in the system of step (3), 90 DEG C of constant temperature stir;
(5) added by the PVP K30 of percentage by weight 5 ~ 8% in the system of step (4), 90 DEG C of constant temperature stir;
(6) added by the PVDF of percentage by weight 20 ~ 25% in the system of step (5), 90 DEG C of constant temperature stir, obtained spinning solution;
(7) delivered to by spinning solution in the closed container of shaping spinning appts, in container, pass into gas, the exit orifice ejection of three on the distributing pipe of spinning solution through being horizontally set on external container concentric diplopore spinning heads, obtains just film;
(8) just film becomes hole slot water-bath through 80 DEG C of grooves that are separated, 60 DEG C of condensate tank(trap)s with 30 DEG C successively, obtains into pore membrane;
(9) pore membrane rolling will be become, 100 DEG C of steam shaping 30min, film forming.
6. the preparation technology of multiplexing type PVDF filter membrane according to claim 5, it is characterized in that: in described step (1) ~ (6) arbitrary step, 90 DEG C of constant temperature mixings time are at least 2h, all add complete in raw material and 12h, the duration summation that 90 DEG C of constant temperature stirs is 48h.
7. the preparation technology of multiplexing type PVDF filter membrane according to claim 5, is characterized in that: be all connected with air exhausting device of bleeding above be separated in described step (8) groove and condensate tank(trap), the water-bath speed of first film is 20m/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114225721A (en) * | 2021-11-26 | 2022-03-25 | 山东东岳高分子材料有限公司 | Safe and environment-friendly method for preparing PVDF porous membrane |
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