CN105344255A - Preparation method for tubular microporous filtering film - Google Patents
Preparation method for tubular microporous filtering film Download PDFInfo
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- CN105344255A CN105344255A CN201510827925.8A CN201510827925A CN105344255A CN 105344255 A CN105344255 A CN 105344255A CN 201510827925 A CN201510827925 A CN 201510827925A CN 105344255 A CN105344255 A CN 105344255A
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- tube
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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
- 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
-
- 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 invention relates to a preparation method for a tubular microporous filtering film. The method concretely comprises the following steps: (1) cleaning the outer surface of a sintered porous tube with uniform pore sizes, and carrying out drying; (2) preparing a film-coating solution according to a certain proportion, then carrying out uniform mixing under stirring, filtering the film-coating solution out, and subjecting the film-coating solution obtained through filtering to vacuum pumping and deaeration inside a material storage tank for subsequent usage; (3) filling a container with the dried sintered porous tube, and subjecting two ends of the tube to sealing treatment; (4) pumping the film-coating solution into the container via a pump and carrying out full filling, and maintaining a constant pressure state for a certain time so that impregnation of the film-coating solution with a certain thickness is realized; and (5) pumping the film-coating solution in the container back to the material storage tank, drawing out the film-coated sintered porous tube, then placing the tube into water, and carrying out soaking so as to obtain the microporous filtering film. The microporous filtering film provided by the invention has excellent filtering accuracy, high strength and long service life, is adaptable to various working conditions and application conditions, and has extensive application prospects in the fields of industrial, municipal and domestic water treatment and liquid separation.
Description
Technical field
The present invention relates to the preparation method of tube-type micropore filter membrane, belong to pellicle separation process technique field, particularly relate to the preparation method of the miillpore filter carrying out aluminum coated steel on sintered porous pipe.
Background technology
At present, membrane separation technique has obtained swift and violent development, and membrane separating maturation applies to the numerous areas such as petrochemical industry, food medicine, mechano-electronic, external coating, bioengineering, industry and domestic use of water process.In the process of film application, fouling membrane is inevitable, especially trade effluent waste water, municipal wastewater process field, so after fouling membrane can rapid regeneration become embrane method can the key issue of further genralrlization application.Therefore, the rapid regeneration method studying resistant to pollution membrane material and film is the focus direction of the application of current film and membrane technology research.
In order to improve resistance tocrocking and the rapid regeneration ability of film, we consider the PVDF material that resistance tocrocking is good on the Material selec-tion of film, rapid regeneration needs the air water backwash of high strength, so by the separation property of film being required to require to separate with self-supporting, just can obtain the intensity of reasonable filtering accuracy and superelevation simultaneously.The molding mode of the outer ultrafiltration of Present Domestic and microfiltration membranes is mainly divided into several as follows: solution phase inversion, pulling method and sintering process.The film that what solution phase inversion can be made have compared with high filtering precision, but higher intensity cannot be obtained, Long-Time Service causes film to occur revealing, and affect result of use, sintering process can obtain high intensity, but cannot obtain higher filtering accuracy, and pulling method is placed in the middle.Be in " a kind of preparation method of contamination-tolerance high-mechanical strength tubular composite membrane and the special equipment " of 02139092.4 at application number, only disclose the film covering method of polyvinyl alcohol material and sintered pipes inner surface.
Summary of the invention
The object of the invention is to overcome the deficiency that existing film product can not have both in precision and intensity, provide one can obtain excellent filtration precision, the preparation method of the PVDF tube-type micropore filter membrane of higher mechanical strength can be obtained again.Improve the antifouling property of film product with this, promote the ability of the contaminated rear rapid regeneration of film product, extend the service life of film.
Technical scheme of the present invention is:
A preparation method for tube-type micropore filter membrane, is characterized in that comprising the following steps:
(1) sintered porous for the porous nickel of purchase tube outer surface is cleaned out, then carry out drying;
(2) according to certain proportioning configuration overlay film liquid, and stir, overlay film liquid is filtered clean, and vacuumizing and defoaming is for subsequent use in storage tank;
(3) dried sintered porous pipe is filled in the container of overlay film, sintered porous pipe two ends encapsulation process;
(4) by overlay film liquid with in pump input pod, and be full of container, keep the pressure constant state of certain hour, make film liquid have certain thickness infiltration;
(5) the overlay film liquid transport pump in container is returned storage tank, extract the sintered porous pipe of overlay film out, then put into water and soak 2-10 hour, obtain miillpore filter.
The pore diameter range of described sintered porous pipe is 1-15 micron.
Described sintered porous pipe baking temperature is 50-90 DEG C, and drying time is 2-6 hour.
Described overlay film liquid is made up of Kynoar, solvent and additive, each component by weight percentage, Kynoar 8-18%, solvent 62-87%, additive 5-20%.
Described Kynoar molecular weight is between 20 ten thousand to 60 ten thousand.
Described solvent is the mixture of one or two or more kinds in dimethyl formamide DMF, dimethylacetylamide DMAc, 1-METHYLPYRROLIDONE NMP.
Described additive is the mixture of one or two or more kinds in PVP K30 (PVP-K30), PVP K90 (PVP-K90), water, PEG400 (PEG400), glycerine.
Pump used in coating process is measuring pump, and after overlay film liquid is full of, the pressure of maintenance is between 0.01-0.1MPa, and the dwell time is between 10-120 second.
Overlay film liquid is 0.5-3mm at the infiltration thickness of sintered porous pipe.
Process in accordance with the present invention can produce the film pipe of the tube-type micropore filter membrane of different application field and different cutoff performance, these film pipes have the filter membrane product that can be packaged into various version, as the membrane module of MBR, shell type, there is extremely wide application space in drinking water treatment, Treated sewage reusing, Industrial Wastewater Treatment and municipal wastewater process field.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Detailed description of the invention
The present invention now describes in detail as follows by reference to the accompanying drawings:
As shown in Figure 1, a kind of preparation method of tube-type micropore filter membrane, carries out according to the following steps:
The first step: the pretreatment of sintered porous pipe: be first that 2 microns of sintered porous tube outer surfaces carry out cleaning by the porous nickel aperture of purchase, remove impurity, clean with the external surface degreasing of acetone further, volatilize after 30 minutes, sintered porous pipe is placed in the baking oven of 60 DEG C, drying time 4 hours;
Second step: add the PVDF needed for overlay film liquid in agitator tank 1, solvent and additive raw material, stir, mixing time 24 hours, then valve (2 is opened, 5, 7), start pump 4, overlay film liquid enters storage tank 8 after filter 6 filters, open vavuum pump simultaneously, open valve 9 to start to vacuumize storage tank 8, until the overlay film liquid in agitator tank 1 is all transported to storage tank 8, then pump 4 is stopped, valve-off (2, 5, 7), but continue to vacuumize storage tank 8, after 30 minutes, valve-off 9 and vavuum pump, the negative pressure state of storage tank 8 is kept to continue deaeration, it is for subsequent use after deaeration completes,
3rd step: sintered porous Guan Yigen mono-good for pretreatment is loaded in the container 12 of overlay film, gap silicone rubber O-ring between sintered porous pipe two ends and container end plate seals, and the end plate 1-2 centimetre at container 12 two of overlay film will be stretched out in the two ends of sintered porous pipe;
4th step: open valve 11 and 13, overlay film liquid is inputted in the container 12 of overlay film by pump 10, until valve 13 has feed liquid to overflow, then valve-off 13.Pay close attention to the pressure state of the container 12 of overlay film simultaneously, during to pressure increase to 0.03-0.05MPa, keep pressure state 30 seconds; Then close pump 10 and valve 11, now overlay film liquid has penetrated into the outer surface of sintered porous pipe completely, and general length of penetration is 1mm;
5th step: open valve 13 and valve 15, starts pump 14, the overlay film liquid in the container 12 of overlay film is re-entered storage tank 8.
6th step: the sintered porous pipe that every root overlay film completes is extracted with nipper plier, silicone rubber O-ring on container end plate can by the remaining overlay film liquid scraped clean of sintered porous tube outer surface, then sintered porous pipe is put into the tank 16 piling water, soak the film pipe of i.e. available tube-type micropore filter membrane after 8 hours.
Following embodiment is undertaken by above-mentioned steps, and just each overlay film liquid raw material configuration is different.
Example 1: take raw material configuration overlay film liquid according to following percentage by weight, molecular weight is the PVDF:DMAc:PVP-K30:PEG400=10%:75%:5%:10% of 300,000, dissolving stirs, according to above-mentioned processing step, the film pipe filtering accuracy of obtained tube-type micropore filter membrane is 0.2um, the pure water flux of unit are reaches 1200L/H (0.1MPa), reaches more than 99.99% to the rejection of microorganism.
Example 2: take raw material configuration overlay film liquid according to following percentage by weight, molecular weight is the PVDF:DMAc:PVP-K30:PVP-K90 of 300,000: glycerine=12%:77%:5%:1%:5%, dissolving stirs, according to above-mentioned processing step, the film pipe filtering accuracy of obtained tube-type micropore filter membrane is 0.1um, the pure water flux of unit are reaches 1000L/H (0.1MPa), reaches more than 99.99% to the rejection of microorganism.
Example 3: take raw material configuration overlay film liquid according to following percentage by weight, molecular weight is the PVDF:DMF:PVP-K90 of 200,000: water: glycerine=8%:87%:2%:1%:2%, dissolving stirs, according to above-mentioned processing step, the film pipe filtering accuracy of obtained tube-type micropore filter membrane is 0.3um, the pure water flux of unit are reaches 900L/H (0.1MPa), reaches more than 99.9% to the rejection of microorganism.
Example 4: take raw material configuration overlay film liquid according to following percentage by weight, molecular weight is the PVDF:DMAc:NMP:PVP-K30:PEG400=18%:25%:37%:5%:15% of 600,000, dissolving stirs, according to above-mentioned processing step, the film pipe filtering accuracy of obtained tube-type micropore filter membrane is 0.05um, the pure water flux of unit are reaches 500L/H (0.1MPa), reaches more than 99.99% to the rejection of microorganism.
Foundation embodiments of the invention are enlightenment above, by above-mentioned description, related personnel completely can in the scope not departing from the technology thought, carry out various change and amendment, the technical scope of this invention is not limited to the content on description, must determine technical scope according to right.
Claims (9)
1. a preparation method for tube-type micropore filter membrane, is characterized in that comprising the following steps:
(1) sintered porous for the porous nickel of purchase tube outer surface is cleaned out, then carry out drying;
(2) according to certain proportioning configuration overlay film liquid, and stir, overlay film liquid is filtered clean, and vacuumizing and defoaming is for subsequent use in storage tank;
(3) dried sintered porous pipe is filled in the container of overlay film, sintered porous pipe two ends encapsulation process;
(4) by overlay film liquid with in pump input pod, and be full of container, keep the pressure constant state of certain hour, make film liquid have certain thickness infiltration;
(5) the overlay film liquid transport pump in container is returned storage tank, extract the sintered porous pipe of overlay film out, then put into water and soak 2-10 hour, obtain miillpore filter.
2. the preparation method of a kind of tube-type micropore filter membrane according to claim 1, is characterized in that: the pore diameter range of described sintered porous pipe is 1-15 micron.
3. the preparation method of a kind of tube-type micropore filter membrane according to claim 1, is characterized in that: described sintered porous pipe baking temperature is 50-90 DEG C, and drying time is 2-6 hour.
4. the preparation method of a kind of tube-type micropore filter membrane according to claim 1, it is characterized in that: described overlay film liquid is made up of Kynoar, solvent and additive, each component by weight percentage, Kynoar 8-18%, solvent 62-87%, additive 5-20%.
5. the preparation method of a kind of tube-type micropore filter membrane according to claim 4, is characterized in that: described Kynoar molecular weight is between 20 ten thousand to 60 ten thousand.
6. the preparation method of a kind of tube-type micropore filter membrane according to claim 4, is characterized in that: described solvent is the mixture of one or two or more kinds in dimethyl formamide DMF, dimethylacetylamide DMAc, 1-METHYLPYRROLIDONE NMP.
7. the preparation method of a kind of tube-type micropore filter membrane according to claim 4, is characterized in that: described additive is the mixture of one or two or more kinds in PVP K30 (PVP-K30), PVP K90 (PVP-K90), water, PEG400 (PEG400), glycerine.
8. the preparation method of a kind of tube-type micropore filter membrane according to claim 1, is characterized in that: pump used in coating process is measuring pump, and after overlay film liquid is full of, the pressure of maintenance is between 0.01-0.1MPa, and the dwell time is between 10-120 second.
9. the preparation method of a kind of tube-type micropore filter membrane according to claim 1, is characterized in that: overlay film liquid is 0.5-3mm at the infiltration thickness of sintered porous pipe.
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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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| CN105344255A true CN105344255A (en) | 2016-02-24 |
| CN105344255B CN105344255B (en) | 2018-01-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | A kind of inner coating surface film technology of tubular composite film |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5487681A (en) * | 1977-12-23 | 1979-07-12 | Mitsubishi Rayon Co Ltd | Preparation of tubular semipermeable membrane |
| JPS62402A (en) * | 1985-06-26 | 1987-01-06 | Kumiai Chem Ind Co Ltd | Industrial disinfectant composition |
| CN102228803A (en) * | 2011-04-19 | 2011-11-02 | 蒋兰英 | Method for preparing hollow fiber composite membrane |
| CN104028108A (en) * | 2014-06-24 | 2014-09-10 | 江苏凯米膜科技股份有限公司 | Method for preparing tubular micro-porous filter membrane |
| CN104289113A (en) * | 2014-10-21 | 2015-01-21 | 武汉尚远环保股份有限公司 | Tubular micro-filtration membrane production equipment |
| CN104785126A (en) * | 2015-04-13 | 2015-07-22 | 淮阴师范学院 | Attapulgite/titanium oxide nano-composite ceramic microfiltration membrane with photocatalytic property and preparation method thereof |
-
2015
- 2015-11-24 CN CN201510827925.8A patent/CN105344255B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5487681A (en) * | 1977-12-23 | 1979-07-12 | Mitsubishi Rayon Co Ltd | Preparation of tubular semipermeable membrane |
| JPS62402A (en) * | 1985-06-26 | 1987-01-06 | Kumiai Chem Ind Co Ltd | Industrial disinfectant composition |
| CN102228803A (en) * | 2011-04-19 | 2011-11-02 | 蒋兰英 | Method for preparing hollow fiber composite membrane |
| CN104028108A (en) * | 2014-06-24 | 2014-09-10 | 江苏凯米膜科技股份有限公司 | Method for preparing tubular micro-porous filter membrane |
| CN104289113A (en) * | 2014-10-21 | 2015-01-21 | 武汉尚远环保股份有限公司 | Tubular micro-filtration membrane production equipment |
| CN104785126A (en) * | 2015-04-13 | 2015-07-22 | 淮阴师范学院 | Attapulgite/titanium oxide nano-composite ceramic microfiltration membrane with photocatalytic property and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | A kind of inner coating surface film technology of tubular composite film |
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| CN105344255B (en) | 2018-01-16 |
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