CN114653224B - Preparation method of hollow fiber membrane of modified support tube - Google Patents
Preparation method of hollow fiber membrane of modified support tube Download PDFInfo
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- CN114653224B CN114653224B CN202210410573.6A CN202210410573A CN114653224B CN 114653224 B CN114653224 B CN 114653224B CN 202210410573 A CN202210410573 A CN 202210410573A CN 114653224 B CN114653224 B CN 114653224B
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- support tube
- aqueous solution
- solution containing
- hollow fiber
- fiber membrane
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- 239000012528 membrane Substances 0.000 title claims abstract description 49
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 38
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 26
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 26
- 238000003618 dip coating Methods 0.000 claims abstract description 21
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920001661 Chitosan Polymers 0.000 claims abstract description 16
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims abstract description 11
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000001070 adhesive effect Effects 0.000 claims abstract description 9
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 238000009987 spinning Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 17
- 238000000576 coating method Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- 238000007598 dipping method Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000004480 active ingredient Substances 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000008093 supporting effect Effects 0.000 description 20
- 238000005266 casting Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000007888 film coating Substances 0.000 description 7
- 238000009501 film coating Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 238000006880 cross-coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920006306 polyurethane fiber Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
-
- 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
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
A preparation method of a hollow fiber membrane of a modified support tube belongs to the technical field of membrane separation. Modifying the surface of a support tube, selecting an aqueous solution containing one or more of Chitosan (CS), polyvinyl alcohol (PVA), dimethylolpropionic acid (BMPA) and N-Aminoethylpiperazine (AEP), performing dip coating treatment on the surface of the support tube, and performing normal spinning to obtain the membrane yarn with improved adhesive force without increasing seepage.
Description
Technical Field
The invention relates to a preparation method of a hollow fiber membrane of a modified support tube, and belongs to the technical field of membrane separation.
Background
In the application of sewage reclamation, the membrane separation technology is mature, economical and feasible and has great potential. However, in the actual use process, the self-supporting hollow fiber membrane has low strength, and the phenomenon of broken wires is easy to occur to influence the water quality, so the hollow fiber membrane with the lining is produced. The hollow fiber membrane with the lining adopts a hollow supporting tube made of nylon, polyester or polyurethane fiber, and the supporting tube is positioned in the inner layer of the hollow fiber membrane, so that the supporting effect is achieved, and the strength of the hollow fiber membrane can be effectively improved. However, since the support tube and the membrane layer are made of different materials (for example, the common support tube is made of PET material, and the common membrane layer is made of PVDF material), and the support tube has high crystallinity, the membrane layer is difficult to firmly combine on the surface thereof, and the membrane layer may easily fall off, thereby affecting the service life of the membrane.
The bonding force between the existing lined hollow fiber membrane layer and the supporting tube mainly depends on the seepage of the membrane layer material on the supporting tube, and the seepage is more and the membrane layer has high adhesive force. However, the method is easy to cause the problems of excessive seepage, blocking of the inner cavity, flux reduction, raw material waste and the like.
Patent application CN104117289a proposes that the hollow fiber membrane support tube is firstly subjected to corona treatment, so that the surface of the hollow fiber membrane support tube is rough, the specific surface area of the support tube is increased, and a transition layer made of the same material as the membrane layer is coated, so that the binding force between the support tube and the membrane layer is larger. The patent has complex implementation process, and the adhesive force is improved by more seepage materials, so that the problems caused by the traditional process cannot be solved.
Patent application CN102430348B describes a method for preparing a PET braided tube/polymer composite hollow fiber membrane, wherein the PET braided tube needs to be immersed with a modifying liquid for a long time, and also needs to be rolled and shaped at a high temperature after immersion, and the process is complex, the time is long, and continuous mass production is difficult.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a hollow fiber membrane of a modified support tube.
A process for preparing the hollow fibrous membrane of modified supporting tube includes such steps as modifying the surface of supporting tube, choosing one or more aqueous solutions containing Chitosan (CS), polyvinyl alcohol (PVA), dimethylolpropionic acid (BMPA) and N-Aminoethylpiperazine (AEP), immersing the surface of supporting tube, coating, spinning, and increasing adhesion.
The dipping coating solution is formed by cross-linking and coupling an acidic aqueous solution containing Chitosan (CS), an aqueous solution containing polyvinyl alcohol (PVA), an aqueous solution containing dimethylolpropionic acid (BMPA) or an aqueous solution containing N-Aminoethylpiperazine (AEP) according to a proportion, and after continuously passing through the dipping solution, the supporting tube can be adhered to the surface of the supporting tube, and the active ingredients can be directly subjected to a film making process after being quickly dried by an online drying device.
The continuous dip coating method is followed by a drying device, and is directly in butt joint with the spinning line.
The dipping coating solution is polyacrylate, cellulose, polyurethane and other organic matters.
The dip coating device, the drying device and the film coating device can form continuous integrated equipment with the spinning line, and can also independently form special supporting tube treatment equipment.
The invention has the advantage of solving the problem that the existing hollow fiber membrane lining (supporting tube) with lining has low binding force with the membrane layer. The continuous dip coating process is simple, the operation speed is high, the continuous dip coating process can be directly connected with a spinning line, the adhesive force is increased through dip coating, meanwhile, the seepage is not increased, and the cost is low.
Drawings
The invention, together with a further understanding of the many of its attendant advantages, will be best understood by reference to the following detailed description, when considered in conjunction with the accompanying drawings, which are included to provide a further understanding of the invention, and the accompanying drawings, illustrate and describe the invention and do not constitute a limitation to the invention, and wherein:
FIG. 1 is a simplified process flow diagram of the present invention.
FIG. 2 is a support tube electron microscopy image before modification.
FIG. 3 is a photograph of the modified support tube electron microscope.
Detailed Description
The invention will be further described with reference to the drawings and examples.
It will be apparent that many modifications and variations are possible within the scope of the invention, as will be apparent to those skilled in the art based upon the teachings herein.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless expressly stated otherwise, as understood by those skilled in the art. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It will be understood that when an element or component is referred to as being "connected" to another element or component, it can be directly connected to the other element or component or intervening elements or components may also be present. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art.
In order to facilitate an understanding of the embodiments, the following description will be given in conjunction with the accompanying drawings, and the various embodiments do not constitute a limitation of the present invention.
Example 1: as shown in figure 1, a hollow fiber membrane preparation device with a modified supporting tube is characterized in that the supporting tube 1 is connected with a precoating groove 2, a drying device 3, a coating device 4, a spinneret plate 5, a gel groove 6 and a filament collecting device 7 through a transmission mechanism.
The preparation method of the hollow fiber membrane of the modified support tube, the impregnating solution providing the adhesive effect is formed by crosslinked coupling of Chitosan (CS) acid aqueous solution or polyvinyl alcohol (PVA) aqueous solution or dimethylolpropionic acid (BMPA) aqueous solution or N-Aminoethylpiperazine (AEP) aqueous solution according to a certain proportion, after the support tube continuously passes through the impregnating solution, the active ingredient can be adhered to the surface of the support tube, the support tube can be quickly dried by an online drying device and then directly enters the membrane preparation process, the adhesive on the surface of the support tube can enhance the adhesive force between the support tube and the membrane layer, and on the other hand, the holes on the support tube can be reduced so as to reduce the seepage and save the raw materials.
A process for preparing the hollow fibrous membrane with modified supporting tube includes such steps as choosing proper precoating solution, continuous immersing coating, treating supporting tube, and preparing membrane on supporting tube. The surface of the support tube after modification is provided with a layer of precoating substance film, the binding force between the crystallinity support tube and the film layer can be improved, the adhesion of the finally prepared hollow fiber film layer is obviously improved, and the modification method is simple to operate, uses less materials and is beneficial to continuous production.
Example 2: a preparation method of a hollow fiber membrane of a modified support tube comprises the following steps:
uniformly mixing one or more of 0.1-1% of Chitosan (CS) acid aqueous solution, 1-5% of polyvinyl alcohol (PVA) aqueous solution, 5-20% of dimethylolpropionic acid (BMPA) aqueous solution and 1-5% of N-Aminoethylpiperazine (AEP) aqueous solution according to a certain proportion, and placing in a precoating tank 2; starting equipment, enabling the support tube 1 to pass through the precoating tank 2 at the speed of 10-70m/min, then passing through the drying device 3, and obtaining a modified support tube after passing through the drying device 3 to the front end of the coating equipment; the casting solution in the film coating device 4 enters a spinneret plate 5 through a feed pump, the support tube after dip coating treatment passes through the spinneret plate 5, the casting solution is uniformly coated on the surface of the support tube after being extruded out of the spinneret plate, and then the hollow fiber film is prepared by gel shaping through a non-solvent gel groove 6 and is collected on a filament collecting device 7.
The support tube disclosed by the invention belongs to a high-crystallinity material, and the surface of the casting solution is difficult to firmly combine, so that the support tube is subjected to precoating treatment before film coating, and the firmness of the film layer is improved through the high adhesive force of precoating substances, the support tube and the film layer.
The following examples all use the same 1.8mm outer diameter support tube.
Example 3: a preparation method of a hollow fiber membrane of a modified support tube comprises the following steps:
the preparation method comprises the steps of mixing an acidic aqueous solution containing 0.1% of chitosan CS, an aqueous solution containing 1% of polyvinyl alcohol PVA and an aqueous solution containing 5% of N-aminoethylpiperazine AEP according to a weight ratio of 6:1:1, enabling a supporting tube to pass through a dipping coating liquid at a speed of 10m/min, and enabling the supporting tube to reach the front end of coating equipment after a drying device is used for preparing the modified supporting tube. And (3) feeding the casting solution into a spinneret plate through a feed pump in the film coating device, extruding the casting solution from the spinneret plate through the spinneret plate, uniformly coating the casting solution on the surface of the support tube, and then carrying out gel forming through a non-solvent gel groove to obtain a hollow fiber film, and collecting the hollow fiber film on a winding wheel, and carrying out treatment and airing. The support tube is shown in fig. 3 and the performance is shown in table 1.
Example 4: a preparation method of a hollow fiber membrane of a modified support tube comprises the following steps:
an aqueous solution containing 3% polyvinyl alcohol PVA, an aqueous solution containing 5% dimethylolpropionic acid BMPA, and an aqueous solution containing 3% N-aminoethylpiperazine AEP were mixed at a weight ratio of 3:2:3 to prepare a dip coating solution, and a support tube was passed through the dip coating solution at a speed of 70m/min, with the remainder being the same as in example 1. The support tube is shown in fig. 3 and the performance is shown in table 1.
Example 5: a preparation method of a hollow fiber membrane of a modified support tube comprises the following steps:
an acidic aqueous solution containing 0.5% of chitosan CS and an aqueous solution containing 2% of polyvinyl alcohol PVA were mixed in a weight ratio of 1:1 to prepare a dip coating solution, and a support tube was passed through the dip coating solution at a speed of 30m/min, with the remainder being the same as in example 4. The support tube is shown in fig. 3 and the performance is shown in table 1.
Example 6: a preparation method of a hollow fiber membrane of a modified support tube comprises the following steps:
the preparation method comprises the steps of (1) taking an aqueous solution containing 10% of dimethylolpropionic acid BMPA and an aqueous solution containing 1% of N-aminoethylpiperazine AEP as dip coating liquid according to a weight ratio of 1:1, enabling a support tube to pass through the dip coating liquid at a speed of 10m/min, and drying the support tube to the front end of coating equipment to obtain a modified support tube; and (3) feeding the casting solution into a spinneret plate through a feed pump in the film coating device, uniformly coating the casting solution on the surface of the support tube through the spinneret plate by using the support tube subjected to dip coating treatment, and then carrying out gel shaping through a non-solvent gel groove to obtain a hollow fiber film, and collecting the hollow fiber film on a wire winding wheel, and carrying out treatment and airing. The support tube is shown in fig. 3 and the performance is shown in table 1.
Example 7: a preparation method of a hollow fiber membrane of a modified support tube comprises the following steps:
the modified support tube is prepared by taking an aqueous solution containing 5% of polyvinyl alcohol PVA and an aqueous solution containing 5% of dimethylolpropionic acid BMPA as dip coating solutions in a weight ratio of 1:5, enabling the support tube to pass through the dip coating solution at a speed of 70m/min, and drying the support tube to the front end of a film coating device. The procedure is as in example 4. The support tube is shown in fig. 3 and the performance is shown in table 1.
TABLE 1
Comparative examples: as shown in figure 2, the casting solution in the film coating device enters the spinneret plate through the feed pump, the casting solution passes through the spinneret plate without any treatment, the casting solution is extruded from the spinneret plate and then uniformly coated on the surface of the support tube, and then the hollow fiber film is obtained through gel shaping of a non-solvent gel groove and is collected on a winding wheel, treated and dried.
As described above, the embodiments of the present invention have been described in detail, but it will be apparent to those skilled in the art that many modifications can be made without departing from the spirit and effect of the present invention. Accordingly, such modifications are also entirely within the scope of the present invention.
Claims (6)
1. A preparation method of a hollow fiber membrane of a modified support tube is characterized in that a dipping coating solution is used for modifying the surface of the support tube, the dipping coating solution is formed by crosslinking and coupling an acidic aqueous solution containing 0.1% of chitosan CS, an aqueous solution containing 1% of polyvinyl alcohol PVA and an aqueous solution containing 5% of N-aminoethylpiperazine AEP according to the weight ratio of 6:1:1, the support tube passes through the dipping coating solution at the speed of 10m/min, dipping coating treatment is carried out on the surface of the support tube, after the support tube continuously passes through the dipping solution, active ingredients can be adhered on the surface of the support tube, after the support tube is dried rapidly by an online drying device, normal spinning is carried out, and finally, membrane filaments with improved adhesive force can be obtained without increasing seepage.
2. The method for preparing a hollow fiber membrane of a modified support tube according to claim 1, wherein the continuous dip coating means is followed by a drying device to directly interface with the spinning line.
3. The method for preparing a hollow fiber membrane with a modified support tube according to claim 1, wherein the preparation method is characterized in that an aqueous solution containing 3% of polyvinyl alcohol PVA, an aqueous solution containing 5% of dimethylolpropionic acid BMPA and an aqueous solution containing 3% of N-aminoethylpiperazine AEP are mixed in a weight ratio of 3:2:3 to prepare a dipping coating solution, and the support tube passes through the dipping coating solution at a speed of 70 m/min.
4. The method for preparing a hollow fiber membrane with a modified support tube according to claim 1, wherein the support tube is passed through the dip coating liquid at a speed of 30m/min by mixing an acidic aqueous solution containing 0.5% chitosan CS and an aqueous solution containing 2% polyvinyl alcohol PVA at a weight ratio of 1:1.
5. The method for producing a hollow fiber membrane of a modified support tube according to claim 1, wherein the support tube is passed through the dip coating liquid at a speed of 10m/min with a weight ratio of 1:1 as the dip coating liquid in an aqueous solution containing 10% dimethylolpropionic acid BMPA and an aqueous solution containing 1% N-aminoethylpiperazine AEP.
6. The method for preparing a hollow fiber membrane of a modified support tube according to claim 1, wherein the support tube is passed through the dip coating liquid at a speed of 70m/min with a weight ratio of 1:5, wherein the ratio is an aqueous solution containing 5% polyvinyl alcohol PVA and an aqueous solution containing 5% dimethylolpropionic acid BMPA.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210410573.6A CN114653224B (en) | 2022-04-19 | 2022-04-19 | Preparation method of hollow fiber membrane of modified support tube |
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| CN202210410573.6A CN114653224B (en) | 2022-04-19 | 2022-04-19 | Preparation method of hollow fiber membrane of modified support tube |
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| CN114653224A (en) | 2022-06-24 |
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