CN113877448A - Preparation process and device of ultrathin composite membrane base membrane - Google Patents
Preparation process and device of ultrathin composite membrane base membrane Download PDFInfo
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- CN113877448A CN113877448A CN202111386772.XA CN202111386772A CN113877448A CN 113877448 A CN113877448 A CN 113877448A CN 202111386772 A CN202111386772 A CN 202111386772A CN 113877448 A CN113877448 A CN 113877448A
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- 239000012528 membrane Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005266 casting Methods 0.000 claims abstract description 43
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 230000001112 coagulating effect Effects 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000005345 coagulation Methods 0.000 claims abstract description 5
- 230000015271 coagulation Effects 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000002344 surface layer Substances 0.000 claims description 9
- 238000004804 winding Methods 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 229920002492 poly(sulfone) Polymers 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000004695 Polyether sulfone Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 229920006393 polyether sulfone Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims 3
- 230000035699 permeability Effects 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract description 5
- 238000007654 immersion Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 abstract 1
- 210000004379 membrane Anatomy 0.000 description 18
- 239000010410 layer Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001223 reverse osmosis Methods 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 210000002469 basement membrane Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000614 phase inversion technique Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
Images
Classifications
-
- 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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- 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
-
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/122—Separate manufacturing of ultra-thin membranes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
The invention discloses a preparation process and a device of an ultrathin composite membrane base membrane, wherein the preparation process comprises the following steps: (1) preparing a film casting solution, (2) pressing and polishing non-woven fabrics, (3) pouring the film casting solution into a film casting liquid tank, (4) rolling the non-woven fabrics after the non-woven fabrics sequentially pass through the film casting liquid tank, a coagulating bath water tank and a cleaning water tank; the preparation device comprises: spinning pretreatment equipment, unreeling equipment, a film casting liquid tank, a coagulating bath water tank, a cleaning water tank and reeling equipment. According to the invention, the existing blade coating preparation process of the base film is changed, so that the upper surface and the lower surface of the non-woven fabric are respectively attached with a layer of extremely thin polymer coating, in the immersion process, part of casting film liquid can permeate into the interior of the non-woven fabric, and after coagulation bath phase conversion, the non-woven fabric and the base film layer are tightly connected and are not easy to peel off, so that the prepared base film is extremely thin in thickness, the water permeability is greatly increased, and the salt rejection rate is not reduced; the composite membrane prepared on the basis of the base membrane has higher water permeability and salt rejection rate.
Description
Technical Field
The invention relates to the technical field of composite film production, in particular to a preparation process and a device of an ultrathin composite film base film.
Background
With the rapid increase of the world population and the continuous aggravation of industrialization, the problem of shortage of drinkable water resources is increasingly obvious. The reverse osmosis technology has lower cost and is environment-friendly, and plays an important role in the water treatment industry.
The reverse osmosis membrane comprises three parts, namely a nonwoven fabric layer, a support layer and a polyamide separation layer. Researchers have been working on improving the composition and structure of polyamide layers in an attempt to improve film performance. However, with the rapid development of reverse osmosis technology, researchers are increasingly aware that reverse osmosis performance is not only closely related to the properties of polyamide separation layers, but also affected by the thickness of the support layer, pore size structure, and the like.
At present, the supporting layer of commercial flat or roll composite membrane mostly adopts a basement membrane prepared by an immersion precipitation phase inversion method, and the technological process comprises the steps of firstly dissolving a polymer (and an additive) in a proper organic solvent to obtain a membrane casting solution, carrying out deaeration treatment, then carrying out blade coating on a non-woven fabric reinforcing layer to form a membrane casting solution coating, carrying out solvent evaporation for a short time in a certain temperature and humidity environment, then entering a coagulating bath for solvent and non-solvent exchange, and curing to form a membrane.
Because the thickness of the base film can greatly influence the water permeability and the salt rejection rate of the composite film, the thinner the thickness is, the larger the water permeability is, but the rejection rate can be obviously reduced, and the mechanical strength is also poorer. Therefore, in order to maintain a high rejection rate in the prior art, the water permeability needs to be sacrificed, so that the thickness of the prepared base film is about 200 μm generally.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provide a preparation process and a device of an ultrathin composite membrane base membrane.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation process of an ultrathin composite membrane base membrane is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing the raw materials of the casting solution, mechanically stirring, standing and defoaming to obtain a clear casting solution for later use;
(2) pressing and polishing the non-woven fabric, and winding the non-woven fabric on a stainless steel guide roller of the unwinding equipment in advance;
(3) pouring the casting solution prepared in the step (1) into a casting solution tank to enable the liquid level of the casting solution to be capable of submerging the upper surface layer of the non-woven fabric;
(4) and enabling the non-woven fabric to pass through a film casting liquid tank at a constant speed, respectively forming coatings with the thickness of 15-30 mu m on the upper surface layer and the lower surface layer of the non-woven fabric, evaporating for 5-20 s at room temperature by using air, then allowing the coatings to enter a coagulating bath water tank for carrying out phase conversion reaction for 30-300 s, then allowing the coatings to enter a cleaning water tank for washing away residual solution, and rolling.
Furthermore, the initial thickness of the non-woven fabric is 100-120 mu m, the thickness of the non-woven fabric after pressing and polishing is 50-60 mu m, and the thickness of the prepared base film is 80-120 mu m.
Furthermore, the raw material components of the casting solution are 14-20% of high molecular polymer, 74-78% of organic solvent and 2-12% of additive.
Further, the high molecular polymer comprises one or more of polysulfone, polyethersulfone, sulfonated polysulfone, polyacrylonitrile and polyvinylidene fluoride, the organic solvent comprises one or more of dimethylformamide, dimethylacetamide, dimethyl sulfoxide and propanol, and the additive comprises one or more of polyethylene glycol, poly (ethylene oxide), nano titanium dioxide and polyvinylpyrrolidone.
The utility model provides a device for preparing ultra-thin complex film base film which characterized in that, includes non-woven fabrics pretreatment equipment and along unreels equipment, casting film cistern, coagulation bath water tank, washing water tank and the rolling equipment that the direction of transfer of non-woven fabrics set gradually.
Further, the length of the casting solution groove is 1-2 m, the width is 0.5-1.2 m, and the height is 0.3-0.8 m.
Further, the inside in casting film cistern is provided with deflector roll one and deflector roll two that parallel respectively, and the groove exit in casting film cistern is provided with deflector roll three and deflector roll four that parallel.
Furthermore, the distance between the first guide roller and the second guide roller and the inner bottom surface of the film casting liquid tank is one third of the depth of the film casting liquid tank, and the distance between the first guide roller and the second guide roller is 0.6-1.6 m.
Furthermore, the distance between the guide roller three and the guide roller four is less than 120 mu m, and the guide rollers rotate reversely under the driving of a motor.
Furthermore, the non-woven fabric pretreatment equipment comprises a grinding machine and a high-efficiency hydraulic machine.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the existing blade coating preparation process of the base film is changed, and a corresponding preparation device is adopted, so that the upper surface and the lower surface of the non-woven fabric are respectively attached with a layer of extremely thin polymer coating, part of casting film liquid can permeate into the non-woven fabric in the immersion process, and the non-woven fabric and the base film layer are tightly connected and are not easy to peel off and fall off after the coagulation bath phase conversion, so that the prepared base film is extremely thin in thickness, the water permeability is greatly increased, and the salt rejection rate is not reduced; the composite membrane prepared on the basis of the base membrane has higher water permeability and salt rejection rate.
Drawings
Fig. 1 is a schematic view showing the structure of an apparatus for manufacturing an ultra-thin composite film-based film according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
(1) Preparing a casting solution: mixing 15% of polysulfone, 75% of dimethylacetamide and 10% of polyvinylpyrrolidone, mechanically stirring, standing and defoaming for 24 hours to obtain a clear casting solution;
(2) pressing the non-woven fabric 10 by a hydraulic press, polishing by a polisher, and winding on a stainless steel guide roller of the unwinding equipment in advance;
(3) pouring the casting solution prepared in the step (1) into a casting solution tank 7 to enable the liquid level of the casting solution to be capable of submerging the upper surface layer of the non-woven fabric 10;
(4) the speed of the motor is adjusted to be 3m/min, the unwinding roller 1 and the winding roller 6 are started simultaneously, the non-woven fabric 10 is driven to pass through the film casting liquid tank 7 at a constant speed, the non-woven fabric is conveyed by the first guide roller 2 and the second guide roller 3 in the tank, the distance between the third guide roller 4 and the fourth guide roller 5 is smaller than 120 microns, the third guide roller 4 rotates anticlockwise, the fourth guide roller 5 rotates clockwise, the non-woven fabric 10 passes through the middle of the first guide roller and the second guide roller, redundant film casting liquid is extruded and removed, coatings with the thicknesses of 15-20 microns are formed on the upper surface layer and the lower surface layer of the non-woven fabric 10 respectively, after the air evaporation is carried out for 10s at room temperature, the non-woven fabric enters the coagulation bath water tank 8 to carry out phase conversion reaction for 100s, then enters the cleaning water tank 9 to wash away residual solution, and finally the non-woven fabric is wound on the winding roller 6 to complete winding.
Comparative example
(1) Preparing a casting solution: mixing 15% of polysulfone, 75% of dimethylacetamide and 10% of polyvinylpyrrolidone, mechanically stirring, standing and defoaming for 24 hours to obtain a clear casting solution;
(2) adjusting the height of the scraper, taking non-woven fabrics as a support body, and pouring a membrane casting solution for membrane scraping when the running speed is 3 m/s;
(3) and the diaphragm is wound after passing through the coagulating bath water tank and the cleaning water tank.
The membrane sheets (base membranes) prepared in example one and comparative example were subjected to the same interfacial polymerization conditions to prepare composite membranes, and the test results were as follows:
as can be seen from the data in the table, the thickness of the base film prepared in the first example is 0.6 times that of the comparative example, and the flux is much higher than that of the comparative example; after the composite membrane is prepared, the flux and the desalination rate are high.
Although the present description is described in terms of embodiments, not every embodiment includes only a single embodiment, and such description is for clarity only, and those skilled in the art should be able to integrate the description as a whole, and the embodiments can be appropriately combined to form other embodiments as will be understood by those skilled in the art.
Therefore, the above description is only a preferred embodiment of the present application, and is not intended to limit the scope of the present application; all changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (10)
1. A preparation process of an ultrathin composite membrane base membrane is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing the raw materials of the casting solution, mechanically stirring, standing and defoaming to obtain a clear casting solution for later use;
(2) pressing and polishing the non-woven fabric, and winding the non-woven fabric on a stainless steel guide roller of the unwinding equipment in advance;
(3) pouring the casting solution prepared in the step (1) into a casting solution tank to enable the liquid level of the casting solution to be capable of submerging the upper surface layer of the non-woven fabric;
(4) and enabling the non-woven fabric to pass through a film casting liquid tank at a constant speed, respectively forming coatings with the thickness of 15-30 mu m on the upper surface layer and the lower surface layer of the non-woven fabric, evaporating for 5-20 s at room temperature by using air, then allowing the coatings to enter a coagulating bath water tank for carrying out phase conversion reaction for 30-300 s, then allowing the coatings to enter a cleaning water tank for washing away residual solution, and rolling.
2. The process for preparing an ultrathin composite film-based film according to claim 1, characterized in that: the initial thickness of the non-woven fabric is 100-120 mu m, the thickness of the non-woven fabric after pressing and polishing is 50-60 mu m, and the thickness of the prepared base film is 80-120 mu m.
3. The process for preparing an ultrathin composite film-based film according to claim 1, characterized in that: the raw material components of the casting solution are 14-20% of high molecular polymer, 74-78% of organic solvent and 2-12% of additive.
4. The process for preparing an ultrathin composite film-based film according to claim 3, characterized in that: the high molecular polymer comprises one or more of polysulfone, polyethersulfone, sulfonated polysulfone, polyacrylonitrile and polyvinylidene fluoride, the organic solvent comprises one or more of dimethylformamide, dimethylacetamide, dimethyl sulfoxide and propanol, and the additive comprises one or more of polyethylene glycol, polyepoxy hexane, nano titanium dioxide and polyvinylpyrrolidone.
5. An apparatus for preparing the ultra-thin composite film base film according to claim 1, comprising a non-woven fabric pretreatment device, and an unwinding device, a film casting liquid tank, a coagulation bath water tank, a cleaning water tank and a winding device which are sequentially arranged along a conveying direction of the non-woven fabric.
6. An apparatus for manufacturing ultra thin composite film based film according to claim 5, characterized in that: the length of the film casting solution groove is 1-2 m, the width is 0.5-1.2 m, and the height is 0.3-0.8 m.
7. An apparatus for manufacturing ultra thin composite film based film according to claim 5, characterized in that: the inside in cast film cistern is provided with parallel deflector roll one and deflector roll two respectively, and the groove exit in cast film cistern is provided with parallel deflector roll three and deflector roll four.
8. An apparatus for manufacturing ultra thin composite film based film according to claim 7, characterized in that: the distance between the first guide roller and the second guide roller and the inner bottom surface of the film casting liquid tank is one third of the depth of the film casting liquid tank, and the distance between the first guide roller and the second guide roller is 0.6-1.6 m.
9. An apparatus for manufacturing ultra thin composite film based film according to claim 7, characterized in that: the distance between the third guide roller and the fourth guide roller is less than 120 mu m, and the third guide roller and the fourth guide roller rotate reversely under the driving of a motor.
10. An apparatus for manufacturing ultra thin composite film based film according to claim 5, characterized in that: the non-woven fabric pretreatment equipment comprises a grinding machine and a high-efficiency hydraulic machine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111386772.XA CN113877448A (en) | 2021-11-22 | 2021-11-22 | Preparation process and device of ultrathin composite membrane base membrane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111386772.XA CN113877448A (en) | 2021-11-22 | 2021-11-22 | Preparation process and device of ultrathin composite membrane base membrane |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09313905A (en) * | 1996-05-23 | 1997-12-09 | Nitto Denko Corp | Polysulfone porous separating membrane |
| CN101239280A (en) * | 2007-11-27 | 2008-08-13 | 北京市射线应用研究中心 | Reinforced microporous filter membrane and method and device for preparing the same |
| CN104324623A (en) * | 2014-03-12 | 2015-02-04 | 唐山曹妃甸海清源科技有限公司 | Composite reverse osmosis basal membrane and preparation method thereof |
| CN108404680A (en) * | 2018-03-09 | 2018-08-17 | 西部宝德科技股份有限公司 | A kind of inorganic-organic composite membrane and preparation method thereof |
-
2021
- 2021-11-22 CN CN202111386772.XA patent/CN113877448A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09313905A (en) * | 1996-05-23 | 1997-12-09 | Nitto Denko Corp | Polysulfone porous separating membrane |
| CN101239280A (en) * | 2007-11-27 | 2008-08-13 | 北京市射线应用研究中心 | Reinforced microporous filter membrane and method and device for preparing the same |
| CN104324623A (en) * | 2014-03-12 | 2015-02-04 | 唐山曹妃甸海清源科技有限公司 | Composite reverse osmosis basal membrane and preparation method thereof |
| CN108404680A (en) * | 2018-03-09 | 2018-08-17 | 西部宝德科技股份有限公司 | A kind of inorganic-organic composite membrane and preparation method thereof |
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Application publication date: 20220104 |