CN105344255B - A kind of preparation method of tube-type micropore filter membrane - Google Patents
A kind of preparation method of tube-type micropore filter membrane Download PDFInfo
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- CN105344255B CN105344255B CN201510827925.8A CN201510827925A CN105344255B CN 105344255 B CN105344255 B CN 105344255B CN 201510827925 A CN201510827925 A CN 201510827925A CN 105344255 B CN105344255 B CN 105344255B
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- overlay film
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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
-
- 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
- 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
-
- 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
- B01D69/04—Tubular membranes
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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
- B01D2323/12—Specific ratios of components used
-
- 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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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of preparation method of tube-type micropore filter membrane, specifically comprise the following steps：(1) by hole, uniformly sintered porous tube outer surface is cleaned out, and is then dried；(2) overlay film liquid is configured according to certain proportioning, and stirred, overlay film liquid filtered totally, and vacuumizing and defoaming is standby in storage tank；(3) dried sintered porous pipe is filled into container, both ends encapsulation process；(4) by overlay film liquid with pump input pod, and container is full of, keeps the pressure constant state of certain time, overlay film liquid is had certain thickness infiltration；(5) the overlay film liquid in container is transmitted back to storage tank with pump, extracts the sintered porous pipe of overlay film out, be then placed in water and soak, you can obtain miillpore filter.The miillpore filter of the present invention has that filtering accuracy is excellent, and intensity is high, service life length, adapts in various operating modes and application conditions, has wide practical use in industrial, municipal and civilian water process and liquid separation field.
Description
Technical field
The present invention relates to the preparation method of tube-type micropore filter membrane, belongs to semi-transparent membrane separation process technical field, more particularly to
The preparation method of the miillpore filter of aluminum coated steel is carried out on sintered porous pipe.
Background technology
At present, membrane separation technique has obtained swift and violent development, and maturation applies to petrochemical industry, food to membrane separating
The numerous areas such as medicine, mechano-electronic, external coating, bioengineering, industry and civilian water process.During film is applied,
Fouling membrane is inevitable, especially trade effluent waste water, municipal wastewater process field, then after fouling membrane can rapid regeneration into
For embrane method can further genralrlization application key issue.Therefore, the rapid regeneration method of resistant to pollution membrane material and film is studied
It is the focus direction of current film application and membrane technology research.
In order to improve the resistance tocrocking of film and rapid regeneration ability, we consider that resistance tocrocking is good in the material selection of film
PVDF materials, rapid regeneration needs the air water backwash of high intensity, then by by the separation property requirement of film and self-supporting requirement
Separate, it is possible to while obtain the intensity of relatively good filtering accuracy and superelevation.The shaping of current ultrafiltration and microfiltration film both at home and abroad
Mode is broadly divided into following several：Solution phase inversion, pulling method and sintering process.What solution phase inversion can be made, which have, relatively exceeds
The film of precision is filtered, but higher intensity can not be obtained, long-term use causes film to be revealed, and influences using effect, sintering process energy
High intensity is obtained, but higher filtering accuracy can not be obtained, pulling method is placed in the middle.In Application No. 02139092.4《One
The preparation method and special equipment of kind contamination-tolerance high-mechanical strength tubular composite membrane》In, only disclose polyvinyl alcohol material and burning
Tie the film covering method of pipe internal surface.
The content of the invention
The purpose of the present invention is to overcome the shortcomings of that existing film product can not have both in precision and intensity, there is provided one kind can obtain
Excellent filtration precision is obtained, and can obtains the preparation method of the PVDF tube-type micropore filter membranes of higher mechanical strength.Film production is improved with this
The antifouling property of product, lifting film product are contaminated the ability of rear rapid regeneration, extend the service life of film.
The technical scheme is that：
A kind of preparation method of tube-type micropore filter membrane, it is characterised in that comprise the following steps：
(1) the porous tube outer surface of hole Even Sintering of purchase is cleaned out, be then dried；
(2) overlay film liquid is configured according to certain proportioning, and stirred, overlay film liquid is filtered totally, and in storage tank
Vacuumizing and defoaming is standby；
(3) dried sintered porous pipe is filled into the container of overlay film, sintered porous pipe both ends and encapsulation process；
(4) by overlay film liquid with pump input pod, and container is full of, keeps the pressure constant state of certain time, there is film liquid
Certain thickness infiltration；
(5) the overlay film liquid in container is transmitted back to storage tank with pump, extracts the sintered porous pipe of overlay film out, be then placed in water
2-10 hours are soaked, obtain miillpore filter.
The pore diameter range of the sintered porous pipe is 1-15 microns.
The sintered porous pipe drying temperature is 50-90 DEG C, and drying time is 2-6 hours.
The overlay film liquid is made up of Kynoar, solvent and additive, each component by weight percentage, polyvinylidene fluoride
Alkene 8-18%, solvent 62-87%, additive 5-20%.
Described Kynoar molecular weight is between 20 ten thousand to 60 ten thousand.
Described solvent is one in dimethylformamide DMF, dimethyl acetamide DMAc, 1-METHYLPYRROLIDONE NMP
Kind or more than two kinds of mixture.
Described additive be PVP K30 (PVP-K30), PVP K90 (PVP-K90),
One or two or more kinds of mixtures in water, polyethylene glycol 400 (PEG400), glycerine.
Pump used be measuring pump in coating process, after overlay film liquid is full of, the pressure of holding be 0.01-0.1MPa it
Between, the dwell time is between the 10-120 seconds.
Overlay film liquid is 0.5-3mm in the infiltration thickness of sintered porous pipe.
Process in accordance with the present invention can produce the tube-type micropore filter membrane of different application field and different cutoff performances
Membrane tube, these membrane tubes have the filter membrane product that can be packaged into various structure types, such as MBR, the membrane module of shell type, in drinking water
Processing, Treated sewage reusing, Industrial Wastewater Treatment and municipal wastewater process field have extremely wide application space.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the present invention.
Embodiment
The present invention is described below in detail in conjunction with accompanying drawing：
As shown in figure 1, a kind of preparation method of tube-type micropore filter membrane, is carried out according to the following steps：
The first step：The pretreatment of sintered porous pipe：It is first 2 microns of sintered porous pipe appearances by the hole uniform pore size of purchase
Face carries out cleaning treatment, goes the removal of impurity, is further cleaned with the external surface degreasing of acetone, more by sintering after volatilizing 30 minutes
Hole pipe is placed in 60 DEG C of baking oven, drying time 4 hours；
Second step：PVDF, solvent and the additive raw material needed for overlay film liquid are added in agitator tank 1, is stirred, is stirred
24 hours time, valve (2,5,7) is then opened, start pump 4, overlay film liquid enters storage tank 8 after the filtering of filter 6, together
Shi Kaiqi vavuum pumps, open valve 9 and start to vacuumize storage tank 8, until the overlay film liquid in agitator tank 1 is all transported to storage
Untill batch can 8, then stop pump 4, close valve (2,5,7), but continue to vacuumize storage tank 8, after 30 minutes, shutoff valve
Door 9 and vavuum pump, the negative pressure state of storage tank 8 is kept to continue deaeration, it is standby after the completion of deaeration；
3rd step：In the container 12 that the sintered porous Guan Yigen mono- pre-processed is fitted into overlay film, sintered porous pipe two
Gap between end and container end plate is sealed with silicone rubber O-ring, and the both ends of sintered porous pipe will stretch out 12 liang of the container of overlay film
1-2 centimetres of the end plate of head；
4th step：Valve 11 and 13 is opened, overlay film liquid is inputted in the container 12 of overlay film by pump 10, until valve 13 has
Untill feed liquid is overflowed, valve 13 is then shut off.The pressure state of the container 12 of overlay film is paid close attention to simultaneously, and 0.03- is risen to pressure
During 0.05MPa, pressure state is kept 30 seconds；Pump 10 and valve 11 are then shut off, now overlay film liquid penetrates into burning completely
The outer surface of antipriming pipe is tied, general penetration depth is 1mm；
5th step：Valve 13 and valve 15 are opened, starts pump 14, the overlay film liquid in the container 12 of overlay film is re-entered into storage
Batch can 8.
6th step：The sintered porous pipe for being completed every overlay film with nipper plier is extracted, the silicone rubber seal on container end plate
Then sintered porous pipe can be put into the tank 16 for piling water by circle by the remaining overlay film liquid scraped clean of sintered porous tube outer surface
In, immersion is the membrane tube of available tube-type micropore filter membrane after 8 hours.
Following embodiment is carried out by above-mentioned steps, and simply each overlay film liquid raw material configuration is different.
Example 1：Raw material configuration overlay film liquid is weighed according to following percentage by weight, molecular weight is 300,000 PVDF：DMAc：
PVP-K30：PEG400=10%：75%：5%：10%, dissolving stirs, and according to above-mentioned processing step, obtained tubular type is micro-
The membrane tube filtering accuracy of hole filter membrane is 0.2um, and the pure water flux of unit area reaches 1200L/H (0.1MPa), to microorganism
Rejection reaches more than 99.99%.
Example 2：Raw material configuration overlay film liquid is weighed according to following percentage by weight, molecular weight is 300,000 PVDF：DMAc：
PVP-K30：PVP-K90：Glycerine=12%：77%：5%：1%：5%, dissolving stirs, according to above-mentioned processing step, system
The membrane tube filtering accuracy of the tube-type micropore filter membrane obtained is 0.1um, and the pure water flux of unit area reaches 1000L/H (0.1MPa),
More than 99.99% is reached to the rejection of microorganism.
Example 3：Raw material configuration overlay film liquid is weighed according to following percentage by weight, molecular weight is 200,000 PVDF：DMF：
PVP-K90：Water：Glycerine=8%：87%：2%：1%：2%, dissolving stirs, according to above-mentioned processing step, obtained pipe
The membrane tube filtering accuracy of type micro-hole filter membrane is 0.3um, and the pure water flux of unit area reaches 900L/H (0.1MPa), to microorganism
Rejection reach more than 99.9%.
Example 4：Raw material configuration overlay film liquid is weighed according to following percentage by weight, molecular weight is 600,000 PVDF：DMAc：
NMP：PVP-K30：PEG400=18%：25%：37%：5%：15%, dissolving stirs, according to above-mentioned processing step, system
The membrane tube filtering accuracy of the tube-type micropore filter membrane obtained is 0.05um, and the pure water flux of unit area reaches 500L/H (0.1MPa),
More than 99.99% is reached to the rejection of microorganism.
It is above enlightenment according to embodiments of the invention, by above-mentioned description, related personnel completely can be not
In the range of deviateing the technology thought, various change and modification are carried out, the technical scope of this invention is not limited to
Content on specification, it is necessary to determine the technical scope according to the scope of the claims.
Claims (5)
1. a kind of preparation method of tube-type micropore filter membrane, it is characterised in that comprise the following steps：
（1）The porous tube outer surface of hole Even Sintering of purchase is cleaned out, is then dried；The sintered porous pipe
Pore diameter range is 1-15 microns;The sintered porous pipe drying temperature is 50-90 DEG C, and drying time is 2-6 hours;
（2）Overlay film liquid is configured according to certain proportioning, and is stirred, overlay film liquid is filtered totally, and is taken out very in storage tank
Empty deaeration is standby；
（3）Dried sintered porous pipe is filled into the container of overlay film, sintered porous pipe both ends and encapsulation process；
（4）By overlay film liquid with pump input pod, and container is full of, keeps the pressure constant state of certain time, film liquid is had necessarily
The infiltration of thickness；Pump used is measuring pump in coating process, and after overlay film liquid is full of, the pressure of holding is 0.01-0.1MPa
Between, the dwell time is between the 10-120 seconds;Overlay film liquid is 0.5-3mm in the infiltration thickness of sintered porous pipe;
（5）Overlay film liquid in container is transmitted back to storage tank with pump, the sintered porous pipe of overlay film is extracted out, is then placed in water and soaks
2-10 hours, obtain miillpore filter.
A kind of 2. preparation method of tube-type micropore filter membrane according to claim 1, it is characterised in that：The overlay film liquid is by gathering
Vinylidene, solvent and additive composition, each component by weight percentage, Kynoar 8-18%, solvent 62-87%, add
Add agent 5-20%.
A kind of 3. preparation method of tube-type micropore filter membrane according to claim 2, it is characterised in that：Described polyvinylidene fluoride
Alkene molecular weight is between 20 ten thousand to 60 ten thousand.
A kind of 4. preparation method of tube-type micropore filter membrane according to claim 2, it is characterised in that：Described solvent is two
One or two or more kinds of mixtures in NMF DMF, dimethyl acetamide DMAc, 1-METHYLPYRROLIDONE NMP.
A kind of 5. preparation method of tube-type micropore filter membrane according to claim 2, it is characterised in that：Described additive is
PVP K30（PVP-K30）, PVP K90（PVP-K90）, water, polyethylene glycol 400
（PEG400）, one or two or more kinds of mixtures in glycerine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510827925.8A CN105344255B (en) | 2015-11-24 | 2015-11-24 | A kind of preparation method of tube-type micropore filter membrane |
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| CN201510827925.8A CN105344255B (en) | 2015-11-24 | 2015-11-24 | A kind of preparation method of tube-type micropore filter membrane |
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| CN105344255B true CN105344255B (en) | 2018-01-16 |
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| CN106268327A (en) * | 2016-09-21 | 2017-01-04 | 苏州凯虹高分子科技有限公司 | A kind of preparation method of high temperature resistant tube type filter membrance |
| CN108684127A (en) * | 2018-04-11 | 2018-10-19 | 上海空间推进研究所 | Emitter wetting method and its dedicated unit |
| CN114307673A (en) * | 2021-12-22 | 2022-04-12 | 杨春波 | Internal coating and surface coating process for tubular composite membrane |
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| JPS5938803B2 (en) * | 1977-12-23 | 1984-09-19 | 三菱レイヨン株式会社 | Manufacturing method of tubular semipermeable membrane |
| JPH06682B2 (en) * | 1985-06-26 | 1994-01-05 | クミアイ化学工業株式会社 | Industrial sterilization composition |
| CN102228803B (en) * | 2011-04-19 | 2013-08-07 | 蒋兰英 | Method for preparing hollow fiber composite membrane |
| CN104028108B (en) * | 2014-06-24 | 2016-02-17 | 江苏凯米膜科技股份有限公司 | A kind of preparation method of tube-type micropore filter membrane |
| CN104289113B (en) * | 2014-10-21 | 2016-08-17 | 武汉尚远环保股份有限公司 | A kind of tube type filter membrance produces equipment |
| CN104785126B (en) * | 2015-04-13 | 2017-05-03 | 淮阴师范学院 | Attapulgite/titanium oxide nano-composite ceramic microfiltration membrane with photocatalytic property and preparation method thereof |
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