CN101670244A - Method for preparing nanofiltration membrane supporting body with gradient holes - Google Patents
Method for preparing nanofiltration membrane supporting body with gradient holes Download PDFInfo
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- CN101670244A CN101670244A CN200910035395A CN200910035395A CN101670244A CN 101670244 A CN101670244 A CN 101670244A CN 200910035395 A CN200910035395 A CN 200910035395A CN 200910035395 A CN200910035395 A CN 200910035395A CN 101670244 A CN101670244 A CN 101670244A
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- 239000012528 membrane Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000001728 nano-filtration Methods 0.000 title abstract description 17
- 239000000919 ceramic Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 238000009826 distribution Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims description 29
- 239000000725 suspension Substances 0.000 claims description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 16
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229920000193 polymethacrylate Polymers 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 230000004907 flux Effects 0.000 abstract description 6
- 239000011230 binding agent Substances 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 230000005484 gravity Effects 0.000 abstract 2
- 238000003825 pressing Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000007569 slipcasting Methods 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 230000010412 perfusion Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for preparing a nanofiltration membrane supporting body with gradient hole structures. The method is characterized in that water, a dispersing agent and a binding agent are added to ceramic powder having a grain size distribution range of 50nm-20microns and a mean grain size of 0.1-10 micron to prepare suspending liquid with good dispersity; then the suspending liquid is stood still (gravity settling), sucked by vacuum, dried, sintered and molded. The method ensures that grains in different grain sizes are deposited according to a sequence from big to small through gravity settling and vacuum sucking so as to obtain the nanofiltration membrane supporting body with the gradient hole structures having high flux, high surface performance (smooth and integrated surface without defects), the surface mean grain size of 50-300nm and certain strength.
Description
Technical field
The present invention relates to a kind of method for preparing nanofiltration membrane supporting body, relate in particular to the method that a kind of preparation has gradient porous ceramic NF membrane supporter.
Background technology
Ceramic membrane is widely used in industries such as chemical industry, medicine, food wastewater processing as a kind of new separation technology.Compare with the industrialized organic NF membrane of the part of respective aperture structure, the preparation difficulty of nanofiltration membrane is very big, the used supporter of nanofiltration membrane (is generally unsymmetric structure at present, the top layer aperture is that the preparation of industrialization technology of 50nm～100nm) is grasped by external a few major company as secret, document adopts above-mentioned commercial supporter about the research of nanofiltration membrane, directly prepares nanofiltration membrane thereon and has only German Inopor company to realize the suitability for industrialized production of nanofiltration membrane (about the about 1nm in aperture) at present in the world.It is that the carrier of 1～5 μ m is a supporter that average pore size is adopted in the preparation of nanofiltration membrane usually, prepares the rete that the aperture is 50nm～100nm by 2～3 layers of transition, prepares the microporous barrier of aperture≤2nm at last on this rete.Because the preparation process of ceramic membrane generally will be through filming-drying-roasting process, this just causes adopting above-mentioned conventional method will prepare 5 tunics at least could finally obtain the nanofiltration membrane of aperture less than 5nm, and this brings great difficulty just for the preparation and the industrial applications of nanofiltration membrane.
The disclosed gradient creamics with ceramic membrane fenestrata of Chinese patent CN1081394, be to be major ingredient by aluminium oxide or silica or titanium dioxide, add clay and feldspar is formulated, through slip casting, heat perfusion, the forming method moulding of extruding, pile up crouch dress and the loading of kiln of lifting mode through wet type drying, precision then, under 1100～1550 ℃ of high temperature, fire and form, the ceramic membrane aperture is 0.1～15 μ m, the porosity 30～50%, thickness are 1～200 μ m, totally 2～10 layers.The hole graded ceramics of this preparation method's preparation is though can obtain graded pore structure, the forming process complexity.
The disclosed Functional Graded Ceramics film of world patent WO9821164, this invention are to utilize colloid unstability technology to obtain Functional Graded Ceramics in polydisperse slurry.The key technology that obtains gradient-structure is to prepare controlled and unsettled or metastable colloid shape suspension that have wide particle diameter.When sedimentation, particle gathers partially because of different generation of particle size, and then obtains porous Functional Graded Ceramics material.The gradient ceramic-film of this preparation method's preparation, the unsettled or metastable colloid shape suspension of needs preparation wide particle diameter needs strict controlled condition, has increased the preparation difficulty.
The supporter of preparing high osmosis energy, high surface property (surperficial low roughness, complete sum zero defect) and enough intensity is preparation nanofiltration membrane basis.The nanofiltration membrane supporting body of present report mainly contains following two kinds and prepares thinking:
1) adopt particle diameter to be distributed in the powder of 1～20 μ m as raw material, adopt dry pressing, slip casting, forming methods such as extrinsion pressing prepare ceramic film support, the carrier aperture of this method preparation is bigger, and preparation will prepare five tunics at least less than the nanofiltration membrane of 5nm on supporter; The supporter pore-size distribution of simultaneously this method preparation is wide, follow-up being coated with cause easily in the membrane process preparation liquid in ooze problem such as rete is imperfect.These have brought very big difficulty all for the preparation of nanofiltration membrane and industrialization;
2) raw material that adopts narrow diameter distribution is as the feedstock production ceramic film support, and the supporter of this method preparation can access high surface property, often needs to adopt powder than small particle diameter as raw material, and the supporter permeation flux that makes is less.As people such as H.Verweij (Mottern, M.L., Chiu, W.V., Warchol, Z.T., Shqau, K., Verweij, H., High-performance membrane supports:A colloidalapproach to the consolidation of coarse particles.international journal of hydrogenenergy.33 (2008) 3903-3914) with average grain diameter is α-Al of 300nm
2O
3The ceramic membrane carrier surface roughness of powder preparation is 30nm, and surface apertures is 70nm, but the permeation flux of nitrogen only has～5.15 * 10-7mol/m at normal temperatures
2SPa is far smaller than the permeation flux 1 * 10-5mol/m of nitrogen that can industrial requirement
2SPa.
Summary of the invention
The objective of the invention is in order to improve that traditional preparation process ceramic film support arts demand is repeatedly filmed etc. not enoughly, and provide a kind of preparation to have the method for gradient porous ceramic NF membrane supporter.
Technical scheme of the present invention is: preparation has the method for gradient porous ceramic NF membrane supporter, and its concrete steps are:
1) be raw material with the ceramic powder, adding entry, to be made into mass fraction be 5%～60% suspension, adds dispersant, plasticizer, sintering aid in suspension, ultrasonic again, obtains the suspension of dispersion treatment; Wherein the addition of plasticizer is 0.1%～3% of a suspension quality; The addition of dispersant is 0.1%～3% of a suspension quality; The addition of sintering aid is 0.1%～5% of a ceramic powder gross mass;
2) suspension with dispersion treatment adds in the mould, leaves standstill, and gets graded ceramics supporter green compact through vacuum draw, drying, the demoulding;
3) green compact are warmed up under the sintering temperature and insulation, cooling makes has gradient porous ceramic NF membrane supporter.
Above-mentioned raw material ceramic powder is aluminium oxide, silica, zirconia, titanium dioxide or carborundum, and particle size distribution range is 50nm～20 μ m, and average grain diameter is 0.1～10 μ m.
Preferred above-mentioned plasticizer is a polyvinyl alcohol, and its molecular weight is 22000～90000g/mol; Preferred above-mentioned dispersant is nitric acid or ammonium polymethacrylate; Preferred above-mentioned sintering aid is any one or a few in zirconia, aluminium oxide, titanium dioxide or the silica.
Preferred steps 1) ultrasonic power is 50～100 watts in, and ultrasonic time is 1～20 minute; Step 2) pressure of vacuum draw is 0.1-0.5bar in; Time of repose is 1～20h; Baking temperature is 40～80 ℃, and be 1～3h drying time.
Heating rate is 1～5 ℃/min in the preferred sintering process; Preferred sintering temperature is 600～1300 ℃, and temperature retention time is 1～5h.
It is 50nm～300nm and ceramic film support with graded pore structure of certain intensity that the present invention one prepares high flux, high surface property (smooth surface, complete sum zero defect), surperficial average pore size the step.
Beneficial effect:
The present invention is the different dispersion effect of powder of particle diameter of varying in size by adding in the suspension dispersant etc., reaching.Micron-sized ceramic powder reaches unstable to be disperseed, and the submicron order ceramic powder reaches stable dispersion.Adopt the method for gravitational settling, by controlling the sedimentation of different big or small size particles, the particle of different size is got off according to descending sequential aggradation, the small size particle of supporter top layer (100nm～1 μ m) forms the supporter good surface properties, the big particle diameter of supporter lower floor (1～20 μ m) particle forms the permeance property that big duct helps improving supporter, thereby the nanofiltration membrane supporting body of preparing with graded pore structure can reach the unification of high surface property and high osmosis energy.Compare with extrinsion pressing with traditional dry pressing, the surface low roughness, surface apertures is evenly distributed, be difficult for producing defective, the supporter for preparing identical surface apertures, this method have a step to make surface apertures are 50nm～300nm, have higher flux, avoid repeating repeatedly to film, drying and sintering process, reduce the characteristics such as difficulty of preparation process.
In sum, the present invention adopts the forming method of gravitational settling and vacuum draw, compare with extrinsion pressing with traditional dry pressing, this method is by the sedimentation of the powder of control different-grain diameter, prepare the high surface property that traditional forming method can not prepare, high-throughout have a gradient porous ceramic film support, reduced preparation condition, for follow-up preparation NF membrane coating process provides good basis.
Description of drawings
Fig. 1 is preparation method's flow chart of gradient porous ceramic film support.
Fig. 2 is surface scan (SEM) photo on the top layer of gradient porous ceramic film support.
The specific embodiment
Embodiment 1:
In this example with α-Al
2O
3(particle size distribution range is 100nm～14.2 μ m to powder, average grain diameter is 0.55 μ m) 50 grams add deionized water 50 gram to be mixed with mass concentration are 50% suspension, add nitric acid as dispersant, regulating pH is 2.0, adds molecular weight and be 22000 polyvinyl alcohol 1.0 grams as binding agent; Add 2.0 gram zirconias as sintering aid; Ultrasonic 10 minutes, suspension is added in the mould, left standstill 10 hours, be to aspirate under the 0.2bar at pressure, drying is 2 hours under 40 ℃; The demoulding gets green compact, and green compact are warming up to 950 ℃ of insulations 3 hours with 2.0 ℃/minute heating rate again, cool off naturally, promptly gets to have the gradient porous ceramic film support; The surface scan on this supporter top layer (SEM) photo as shown in Figure 1.
Embodiment 2:
In this example with α-Al
2O
3(particle size distribution range is 100nm～4.0 μ m to powder, average grain diameter is 0.8 μ m) 40 grams add deionized water 60 gram to be mixed with mass concentration are 40% suspension, add ammonium polymethacrylate 0.2 gram as dispersant, add molecular weight and be 55000 polyvinyl alcohol 2.3 grams as binding agent; Add zirconia 1.6 grams as sintering aid; Ultrasonic 10 minutes, suspension is added in the mould, left standstill 15 hours, be to aspirate under the 0.2bar at pressure, drying is 2 hours under 40 ℃; The demoulding gets green compact, and green compact are warming up to 1150 ℃ of insulations 1 hour with 1.5 ℃/minute heating rate, cool off naturally, promptly gets to have the gradient porous ceramic film support.
Embodiment 3:
(particle size distribution range is 100nm～4.78 μ m with Zirconium powder, average grain diameter is 0.27 μ m) 40 grams add deionized water 460 gram to be mixed with mass concentration are 8% suspension, add ammonium polymethacrylate 0.2 gram as dispersant, add molecular weight and be 55000 polyvinyl alcohol 2.3 grams as binding agent; Add zirconia 1.6 grams and aluminium oxide 10 grams as sintering aid; Ultrasonic 10 minutes, suspension is added in the mould, left standstill 15 hours, be to aspirate under the 0.1bar at pressure, drying is 1 hour under 70 ℃; The demoulding gets green compact, and green compact are warming up to 1150 ℃ of insulations 1 hour with 1.5 ℃/minute heating rate, cool off naturally, promptly gets to have the gradient porous ceramic film support.
Claims (6)
1. preparation has the method for gradient porous ceramic NF membrane supporter, and concrete steps are:
1) be raw material with the ceramic powder, adding entry, to be made into mass fraction be 5%～60% suspension, adds dispersant, plasticizer, sintering aid in suspension, ultrasonic again, obtains the suspension of dispersion treatment; Wherein the addition of plasticizer is 0.1%～3% of a suspension quality; The addition of dispersant is 0.1%～3% of a suspension quality; The addition of sintering aid is 0.1%～5% of a ceramic powder gross mass;
2) suspension with dispersion treatment adds in the mould, leaves standstill, and gets graded ceramics supporter green compact through vacuum draw, drying, the demoulding;
3) green compact are warmed up under the sintering temperature and insulation, cooling makes has gradient porous ceramic NF membrane supporter.
2. method according to claim 1 is characterized in that the raw material ceramic powder is aluminium oxide, silica, zirconia, titanium dioxide or carborundum, and particle size distribution range is 50nm～20 μ m, and average grain diameter is 0.1～10 μ m.
3. method according to claim 1 is characterized in that described plasticizer is a polyvinyl alcohol, and its molecular weight is 22000～90000g/mol; Described dispersant is nitric acid or ammonium polymethacrylate; Described sintering aid is any one or a few in zirconia, aluminium oxide, titanium dioxide or the silica.
4. method according to claim 1 is characterized in that ultrasonic power is 50～100 watts in the step 1), and ultrasonic time is 1～20 minute; Step 2) pressure of vacuum draw is 0.1-0.5bar in; Time of repose is 1～20h; Baking temperature is 40～80 ℃, and be 1～3h drying time.
5. method according to claim 1 is characterized in that sintering temperature is 600～1300 ℃, and temperature retention time is 1～5h.
6. method according to claim 1 is characterized in that heating rate is 1～5 ℃/min in the sintering process.
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Cited By (18)
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| CN101985084A (en) * | 2010-11-18 | 2011-03-16 | 南京工业大学 | Preparation method for ceramic Ti-Al alloy composite membrane |
| CN103566774A (en) * | 2012-07-27 | 2014-02-12 | 佛山市南海区西樵金刚科技有限公司 | Inorganic film support and making method thereof |
| CN104587846A (en) * | 2014-12-24 | 2015-05-06 | 长安大学 | Method for preparing porous ceramic filter membrane by low-temperature sintering |
| CN104987120A (en) * | 2015-07-21 | 2015-10-21 | 江苏九天高科技股份有限公司 | Molecular sieve membrane support body preparation method |
| CN105251375A (en) * | 2015-11-19 | 2016-01-20 | 肖汉宁 | Preparation method of multilayered gradient ceramic membrane |
| CN107349800A (en) * | 2017-08-14 | 2017-11-17 | 苏州博清高新材料有限公司 | A kind of ceramic membrane of bore diameter gradient distribution and preparation method thereof |
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081394A (en) * | 1992-07-15 | 1994-02-02 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Gradient creamics with ceramic membrane fenestrata |
| US6225246B1 (en) * | 1996-11-12 | 2001-05-01 | National Research Council Of Canada | Functionally gradient ceramic structures |
-
2009
- 2009-09-27 CN CN2009100353958A patent/CN101670244B/en active Active
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| CN113173782A (en) * | 2021-04-23 | 2021-07-27 | 深圳市基克纳科技有限公司 | Composition and porous ceramic atomizing core containing micropores with gradient distribution |
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