CN112295414A - Three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation - Google Patents
Three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 86
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 53
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 51
- 239000010935 stainless steel Substances 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000926 separation method Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 31
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 25
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 16
- 239000002105 nanoparticle Substances 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 238000007598 dipping method Methods 0.000 claims description 6
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000003618 dip coating Methods 0.000 claims description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 13
- 235000019198 oils Nutrition 0.000 description 13
- 239000000463 material Substances 0.000 description 9
- 230000014759 maintenance of location Effects 0.000 description 7
- 230000004907 flux Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229920005597 polymer membrane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000010499 rapseed oil Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000614 phase inversion technique Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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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
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- 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
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation, which comprises the steps of sintering a three-channel stainless steel hollow fiber membrane and enabling the inner wall of the three-channel stainless steel hollow fiber membrane to contain TiO2And (3) sintering the three-channel stainless steel hollow fiber membrane. The invention has the following advantages: the inner surface has good hydrophilicity, high underwater oleophobic property and high mechanical strength; in the practical application process, the membrane is not easy to damage, and has excellent oil-water separation performance, anti-pollution capability in long-term operation and cycle performance. Therefore, the method has great application value in the practical application of oil-water separation.
Description
Technical Field
The invention relates to a three-channel stainless steel hollow fiber membrane, in particular to a three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation.
Background
With the aggravation of petroleum pollution, an oil-water separation technology becomes more and more important, and a functional material for effectively treating oil-containing wastewater is concerned. Therefore, various novel materials and oil/water separation methods have been intensively studied. At present, the oil-water separation material can be divided into a filter material and an absorbent material by a separation method so far. The filtering material applied to oil-water separation comprises: wire mesh, fabric, film, etc. Due to their larger pore size, meshes and fabrics are commonly used to separate free oil/water mixtures. While some meshes are also useful for the separation of emulsified oil/water mixtures, membrane materials are more suitable for the separation of highly emulsified oil/water mixtures, particularly surfactant-stabilized emulsions, because of their smaller pore size. Currently, most oil/water separation membranes use polymer membranes and ceramic membranes. Polymer membranes, although widely studied for their high flux and separation efficiency. It is still limited to practical applications due to poor chemical stability and antifouling ability. However, the ceramic membrane has poor mechanical strength and poor cycle performance, which still causes great problems. Thus, stainless steel membranes for oil/water separation show great potential, since the mechanical stability and fouling resistance of stainless steel are much higher than those of ceramics and polymers, respectively.
To improve the oil/water separation performance, much of the current research has focused on hydrophilic and oleophobic modification of membranes. To date, surface chemical modification, geometric control and hybrid doping have been commonly used to improve both of these features. Due to the nanometer TiO2The inherent hydrophilicity and surface roughness of particles has attracted considerable attention. Shi et al (J.Membr.Sci.506(2016)60-70) by direct binding to TiO2The nanoparticles produce high water permeation flux membranes on polyvinylidene fluoride (PVDF) membranes, and the produced oil/water separation membranes also exhibit excellent circulation and fouling resistance. Zhang et al (appl.Surf.Sci.458(2018)157-165) adopt magnetron sputtering and hydrothermal oxidation methods to prepare super-hydrophilic and underwater super-oleophobic TiO2/Al2O3A composite membrane. Effectively improves the oil/water separation efficiency and obviously reduces the surface pollution degree. Chang et al (J.Membr.Sci.456(2014)128-133) use nano TiO by in situ precipitation2The coating modifies a commercial ceramic membrane that has good repellency to stable oil-in-water emulsions. Undoubtedly, nano TiO2The particles show great potential in oil/water separation. Furthermore, TiO2Such as thermal stability, chemical stability and good adhesion to metal substrates, can also take full advantage of the stainless steel film.
Currently, most commercial membranes are flat sheet membranes and single channel hollow fiber membranes. Compared to these two membranes, three-channel hollow fiber (TCHF) membranes not only have higher packing density, surface area to volume ratio than flat sheet membranes, but also have higher luminal surface area and membrane strength than single-channel hollow fiber membranes. TCHF films are therefore of great interest because of their potentially new properties. Lu et al (J.Membr.Sci.514(2016) 165-175) developed a PVDF triple channel hollow fiber membrane with better mechanical strength than single channel membranes. After the Teflon AF2400 coating, the membrane material shows better stability, and the rejection rate of the membrane material for seawater desalination application at 60 ℃ is 99.99%. Lee et al (j.membr. sci.489(2015)64-72) prepared alumina three channel hollow fiber membranes by the phase inversion method, which had higher breaking load and water permeation flux than single channel hollow fiber membranes. However, to date, the fabrication of superhydrophilic three-channel stainless steel hollow fiber (TCSSHF) membranes has not been studied systematically.
Disclosure of Invention
The invention provides a three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation2The nano particles and the polyvinyl alcohol coating effectively improve the hydrophilicity and the mechanical property of the three-channel stainless steel hollow fiber membrane, have excellent separation performance on various oil-water systems, and have practical application value in the separation process of the oil-water systems.
The technical scheme of the invention is to prepare coating liquid; adopts a dipping and pulling method to coat TiO on the inner wall of a three-channel stainless steel hollow fiber membrane2Nanoparticles and polyvinyl alcohol coatings; sintering of TiO in muffle furnace2The method for controlling the structure of the three-channel stainless steel hollow fiber membrane applied to oil-water separation finally comprises the following specific steps:
(1) preparation of a solution containing TiO2Coating the inner wall of a three-channel stainless steel hollow fiber membrane with TiO by a dipping and pulling method2A nanoparticle layer;
(2) TiO prepared in the step (1)2Airing the three-channel stainless steel hollow fiber membrane with the inner wall coating for 12-48 hours at room temperature, preferably 24 hours;
(3) preparing a polyvinyl alcohol solution, and coating the polyvinyl alcohol solution on the inner wall of the three-channel stainless steel hollow fiber membrane treated in the step (2);
(4) and (4) sintering the three-channel stainless steel hollow fiber membrane prepared in the step (3) in a muffle furnace.
Further, TiO in the coating solution used in the step (1)2The content of the nano particles is 0-15 wt.%; preferably 2.5 wt.%.
Furthermore, piperazine with the content of 0.1-1.0 wt.% is added into the coating solution used in the step (1).
Further, the dip-coating method used in the step (1) is used for coating TiO2The dipping time of the nano particles is 0-30 s.
Further, the pulling rate in the step (2) is 50 cm/min.
Further, the concentration of the polyvinyl alcohol coating liquid used in the step (3) is 0.1-1.0 wt.%.
Further, the compound used in step (5) has TiO2The sintering conditions of the three-channel stainless steel hollow fiber membrane of the nano-particle inner wall coating are as follows: sintering at 400-600 ℃ for 1-3 hours.
The invention also provides a three-channel stainless steel hollow fiber membrane obtained by the three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation.
According to the method, the prepared three-channel stainless steel hollow fiber membrane applied to oil-water separation is used for separating an oil/water emulsion system.
The invention has the beneficial technical effects that:
according to the three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation, the TiO2 nano particle coating is uniform in thickness, is tightly combined with a stainless steel base membrane, is smooth and complete in membrane surface, has no defects, has excellent hydrophilicity and oleophobicity, and is not easy to damage in the actual operation and assembly preparation process because the TiO2 nano particle coating is arranged on the inner wall of the three-channel stainless steel hollow fiber membrane.
The three-channel stainless steel hollow fiber membrane applied to oil-water separation has good inner surface hydrophilicity, high underwater oleophobic property and high mechanical strength; in the practical application process, the membrane is not easy to damage, and has excellent oil-water separation performance, anti-pollution capability in long-term operation and cycle performance. Therefore, the method has great application value in the practical application of oil-water separation.
Drawings
FIG. 1 is a scanning electron microscope image (full section) of a three-channel stainless steel hollow fiber-based membrane;
FIG. 2 scanning electron micrograph (inner surface) of three-channel stainless steel hollow fiber-based film;
FIG. 3 is a scanning electron microscope image (section part) of a three-channel stainless steel hollow fiber-based membrane;
FIG. 4 inner wall TiO of example 12Scanning electron micrographs (inner surfaces) of three-channel stainless steel hollow fiber membranes;
FIG. 5 inner wall TiO of example 12Scanning electron micrographs (local internal surface) of a three-channel stainless steel hollow fiber membrane;
FIG. 6 inner wall TiO of example 12Scanning electron micrographs (sections partial) of the three-channel stainless steel hollow fiber membrane.
Detailed Description
The formula for calculating the membrane flux is shown in (1)
Wherein J is the flux of the membrane (L/(m)2H)), V is the volume (L) of the collected permeate, and A is the effective area (m) of the membrane2) And T is the time (h) required to collect a volume of permeate.
The method for calculating the retention performance of the membrane is shown in (2).
Wherein R is the rejection of the membrane, CpConcentration on the permeate side, CfIs the concentration on the feed side.
The oil-water concentration is measured by an ultraviolet-visible spectrophotometer, and then the rejection rate is calculated. All membranes were measured 3 times and the results were averaged.
The following provides a TiO-containing composition of the present invention2The specific embodiment of the three-channel stainless steel hollow fiber membrane coated on the inner wall of the nano particle.
Example 1
By mixing nano TiO2Preparation of TiO by dispersing particles in PIP solution2A coating suspension. Firstly, the TCSSHF membrane is vertically fixed, and the lower end of the membrane is connected by a hose. Firstly, the first step is toContaining 2.5 wt.% of nano TiO2The coating suspension of the particle content was pumped into the lumen side, the suspension was pumped by a peristaltic pump at a rate of 50cm/min until the lumen was filled, and after 5s of immersion, the suspension was pumped at the same rate.
After drying for 24h at ambient temperature, coating 0.5 wt% PVA solution on the inner wall of the membrane by a similar method, calcining for 2h at 500 ℃ to obtain TiO2Three-channel stainless steel hollow fiber membrane coated on the inner wall of the nano-particles. And (3) placing the prepared membrane module into a component, and immersing the component into deionized water to be tested.
The retention was tested with 5000ppm rape oil/water emulsion at an operating temperature of 25 ℃ and an operating pressure of 0.10 MPa. The membrane has a test flux of 760L/(m)2H), the retention rate is 99.8%.
Examples 2 to 5
The procedure of example 1 was followed except that the dipping times were 0s, 10s, 20s and 30s, and the retention performance was measured by using 5000ppm of rape oil/water emulsion at an operating temperature of 25 ℃ and an operating pressure of 0.10 MPa. The results are given in the following table:
examples 6 to 10
The same procedure as in example 1 was followed except that the coating suspension had a particle content of 0 wt.%, 1.0 wt.%, 5.0 wt.%, 10 wt.% and 15 wt.%, and the retention properties were measured with a 5000ppm rapeseed oil/water emulsion at an operating temperature of 25 ℃ and an operating pressure of 0.10 MPa. The results are given in the following table:
examples 11 to 14
Except that the test raw material liquid was changed to 5000ppm vegetable oil, pump oil, chloroform, and n-hexane emulsion, and the operation pressure was changed to 0.05MPa, the procedure was the same as in example 1, and the retention property was tested at an operation temperature of 25 ℃. The results are given in the following table:
examples 15 to 17
The procedure of example 1 was followed except that the operating pressure was changed to 0.20MPa and 0.30MPa, and the retention was measured at an operating temperature of 25 ℃ with a vegetable oil/water emulsion of 5000 ppm. The results are given in the following table:
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations should also be regarded as being within the protection scope of the present invention.
Claims (9)
1. A three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation is characterized by comprising the following specific steps:
(1) preparation of a solution containing TiO2Coating the inner wall of a three-channel stainless steel hollow fiber membrane with TiO by a dipping and pulling method2A nanoparticle layer;
(2) TiO prepared in the step (1)2Airing the three-channel stainless steel hollow fiber membrane with the inner wall coating for 12-48 hours at room temperature;
(3) preparing a polyvinyl alcohol solution, and coating the polyvinyl alcohol solution on the inner wall of the three-channel stainless steel hollow fiber membrane treated in the step (2);
(4) and (4) sintering the three-channel stainless steel hollow fiber membrane prepared in the step (3) in a muffle furnace.
2. The method for controlling the structure of the three-channel stainless steel hollow fiber membrane applied to oil-water separation according to claim 1, wherein the TiO in the coating solution used in the step (1) is TiO2The content of the nano particles is 0 wt.% to 15 wt.%.
3. The method for controlling the structure of the three-channel stainless steel hollow fiber membrane applied to oil-water separation according to claim 1, wherein piperazine with the content of 0.1-1.0 wt.% is added to the coating solution used in the step (1).
4. The method for controlling the structure of a three-channel stainless steel hollow fiber membrane applied to oil-water separation according to claim 1, wherein the dip-coating method used in the step (1) is a TiO coating method2The dipping time of the nano particles is 0-30 s.
5. The method for controlling a three-channel stainless steel hollow fiber membrane structure applied to oil-water separation as claimed in claim 1, wherein the pulling rate in the step (2) is 50 cm/min.
6. The method for controlling the structure of the three-channel stainless steel hollow fiber membrane applied to oil-water separation as claimed in claim 1, wherein the concentration of the polyvinyl alcohol coating solution used in the step (3) is 0.1-1.0 wt.%.
7. The method for controlling a three-channel stainless steel hollow fiber membrane structure applied to oil-water separation of claim 1, wherein TiO is added in the step (5)2The sintering conditions of the three-channel stainless steel hollow fiber membrane of the nano-particle inner wall coating are as follows: sintering at 400-600 ℃ for 1-3 hours.
8. A three-channel stainless steel hollow fiber membrane obtained by the three-channel stainless steel hollow fiber membrane structure control method applied to oil-water separation as recited in any one of claims 1 to 7.
9. Use of the three-channel stainless steel hollow fiber membrane for oil-water separation according to claim 8 for separation of oil/water emulsion system.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116239182A (en) * | 2023-03-17 | 2023-06-09 | 湖南长科诚享石化科技有限公司 | Oil removal device, oil-water-gas separation system and method |
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| WO2018230786A1 (en) * | 2017-06-13 | 2018-12-20 | 김정학 | Dehumidifying hollow fiber membrane, dehumidifying module using same, method for manufacturing dehumidifying hollow fiber membrane, and humidity-adjustable air purifier using hollow fiber membrane |
| WO2019122828A1 (en) * | 2017-12-19 | 2019-06-27 | G2O Water Technologies Limited | Membrane |
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2019
- 2019-07-25 CN CN201910678650.4A patent/CN112295414A/en active Pending
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| WO2018230786A1 (en) * | 2017-06-13 | 2018-12-20 | 김정학 | Dehumidifying hollow fiber membrane, dehumidifying module using same, method for manufacturing dehumidifying hollow fiber membrane, and humidity-adjustable air purifier using hollow fiber membrane |
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| Title |
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| CN116239182A (en) * | 2023-03-17 | 2023-06-09 | 湖南长科诚享石化科技有限公司 | Oil removal device, oil-water-gas separation system and method |
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