CN114307688B - Membrane thickness gradient distribution ceramic filtering membrane and preparation method thereof - Google Patents
Membrane thickness gradient distribution ceramic filtering membrane and preparation method thereof Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 131
- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- 238000009826 distribution Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001914 filtration Methods 0.000 title claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 14
- 230000004907 flux Effects 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005488 sandblasting Methods 0.000 claims description 28
- 239000012188 paraffin wax Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 102220043159 rs587780996 Human genes 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000009295 crossflow filtration Methods 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 238000005422 blasting Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 238000002347 injection Methods 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 238000010345 tape casting Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000005266 casting Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000008676 import Effects 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- B01D71/02—Inorganic material
Abstract
The invention discloses a ceramic filter membrane with gradient distribution of membrane thickness and a preparation method thereof, wherein the pure water flux under the pressure of 0.1MPa is 2100-2800LMH, the ceramic filter membrane comprises a ceramic membrane support body and a ceramic membrane layer arranged on the surface of the ceramic membrane support body, the thickness of the ceramic membrane layer is gradually reduced along the direction from a feed end to a discharge end, the thickness is gradually reduced from 35-55 mu m to 8-25 mu m, the porosity of the ceramic membrane layer is 32-40%, and the pore diameter is 80-300nm. According to the invention, the position with large thickness of the ceramic membrane layer is used as a feeding end, the filtering resistance is large, the position with small thickness of the ceramic membrane layer is used as a discharging end, and the filtering resistance is small, so that the problems of large pressure of a feeding port, small pressure of a discharging port, uneven membrane flux and membrane pollution and low effective utilization rate of the membrane in cross-flow filtration are solved.
Description
Technical Field
The invention belongs to the technical field of membrane separation materials, and particularly relates to a membrane thickness gradient distribution ceramic filter membrane and a preparation method thereof.
Background
The importance of membrane technology and membrane applications in technological innovation and national economic development has become more and more evident, and membranes and membrane processes have been highly valued by countries throughout the world at present. Compared with the traditional polymer separation membrane material, the ceramic membrane has good chemical stability, and can resist acid, alkali and organic solvents; the mechanical strength is high, and the back flushing can be realized; the antimicrobial capability is strong; high temperature resistance; narrow pore size distribution, high separation efficiency and the like, and is widely applied in the fields of food industry, bioengineering, environmental engineering, chemical industry, petrochemical industry, metallurgical industry and the like.
Commercial ceramic membranes generally have three-layer structures (a porous supporting layer, a transition layer and a separation layer) and are asymmetrically distributed, the pore size of the ceramic membranes is different from 0.8nm to 1 mu m, and the filtration precision covers the micro-filtration, ultra-filtration and nano-filtration levels. The support of the ceramic membrane is usually produced by extrusion molding, slip casting, gel casting and the like, and the transition membrane layer and the filter membrane layer are usually prepared by conventional preparation methods such as dip coating, spraying, casting, sol-gel and the like. The ceramic membrane layer prepared by the conventional method has relatively uniform porosity and membrane layer thickness. However, in practical applications, the ceramic membrane usually adopts a cross-flow filtration mode, and the liquid feed liquid in the membrane filtration process can be divided into feed liquid, concentrated liquid and penetrating liquid. The feed liquid pressure of membrane feed liquid import position is greater than the concentrated hydraulic pressure force of membrane exit position, leads to the flow and the pollution speed of membrane feed liquid import position to be greater than membrane feed liquid exit position far away, and along membrane pipe length direction, by feed inlet to discharge gate, osmotic pressure reduces gradually, and the infiltration flow reduces gradually, and the pollution speed reduces gradually. This just leads to the membrane pipe ejection of compact uneven, and membrane tube rear end membrane filtration efficiency is low, the problem of the front end serious pollution.
CN 101182233A discloses a ceramic membrane, which is prepared by mixing ceramic powder with solvents such as ammonium polyacrylate, etc., and by adopting a tape casting method, the thickness of the membrane is controlled by a scraper, and after low-temperature freezing, the membrane is in-situ formed into a ceramic membrane with a gradient distribution of membrane thickness. However, the method has complex process and great operation difficulty, the solvent for preparing the slurry has certain toxicity and pollutes the environment, and the film thickness can not be accurately controlled due to the influence of the self-dispersibility and the fluidity of the high-solid-content ceramic slurry. CN 101182233A discloses a method for preparing a ceramic membrane with pore gradient distribution along the thickness direction of the membrane by using photocuring rapid molding in combination with gel-casting molding, but the method has complex process and high preparation cost, and the prepared ceramic membrane cannot solve the problems of large pressure at the feed inlet, small pressure at the discharge outlet, uneven membrane flux and membrane pollution, and low effective utilization rate of the membrane in cross-flow filtration.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a ceramic filter membrane with gradient distribution of membrane thickness.
The invention also aims to provide a preparation method of the film thickness gradient distribution ceramic filter membrane.
The technical scheme of the invention is as follows:
the ceramic filter membrane with the gradient distribution of the membrane thickness has the pure water flux of 2100-3200LMH under the pressure of 0.1MPa, and comprises a ceramic membrane support body and a ceramic membrane layer arranged on the surface of the ceramic membrane support body, wherein the thickness of the ceramic membrane layer is gradually reduced along the direction from a feed end to a discharge end, the thickness is gradually reduced from 35-55 mu m to 8-25 mu m, the porosity of the ceramic membrane layer is 32-40%, and the pore diameter is 80-300nm.
The preparation method of the ceramic filter membrane with the membrane thickness gradient distribution comprises the following steps:
(1) Coating a paraffin film layer with the thickness of 40-70 mu m on the ceramic membrane support body, and naturally cooling;
(2) Heating ceramic powder particles for preparing the ceramic film layer to 80-100 ℃, and then spraying the ceramic powder particles on the paraffin film layer by using a hot air sand blasting device, wherein under the condition of fixed spraying pressure and moving speed, the sand blasting flow of the hot air sand blasting device is from 3m to 6m within 120s along the direction from one end to the other end of the ceramic film support body 3 The speed of the reaction is increased to 8 to 15m at a constant speed 3 /h；
(3) And (3) sintering the material obtained in the step (2) to obtain the ceramic filter membrane with the gradient distribution of membrane thickness.
In a preferred embodiment of the invention, the ceramic membrane support has a pore size D50=1-8 μm.
In a preferred embodiment of the invention, the ceramic membrane layer is made of ceramic powder particles with a D50=0.3-0.8 μm.
In a preferred embodiment of the invention, the paraffin in the paraffin film layer has a melting point of 60 to 115 ℃.
Further preferably, the temperature of the hot air blasting device is 45-85 ℃.
In a preferred embodiment of the present invention, the jet pressure of the hot air blasting device is 1.8 to 2.2MPa.
In a preferred embodiment of the present invention, the moving speed of the hot blast blasting device is 0.008 to 0.012m/s.
In a preferred embodiment of the invention, the sintering temperature is between 1100 and 1700 ℃.
Further preferably, the sintering time is 2-6h.
The invention has the beneficial effects that:
1. the invention solves the problems of large pressure of a feed inlet, small pressure of a discharge outlet, uneven membrane flux and membrane pollution and low effective utilization rate of the membrane in cross flow filtration.
2. The preparation method can deposit the ceramic film layer with the thickness gradient distribution along the length direction of the film on the ceramic film support.
3. The preparation method has the advantages of simple process and equipment, easy automation control, high production efficiency, no toxic auxiliary agent, safety and reliability.
4. The preparation method can directly form the separation film layer on the ceramic film support without a transition film layer in the traditional process, thereby further improving the production efficiency and greatly reducing the production cost.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
A 45 μm paraffin (melting point, 90 ℃) film layer was coated on an alumina ceramic film support with a pore diameter D50=3 μm by a tape casting method and naturally cooled, and then alumina ceramic powder particles (D50 =0.6 μm) for preparing the film layer were heated to 65 ℃ and sprayed on the paraffin film layer by a hot air (60 ℃) blasting device. The moving speed (0.01 m/s) and the injection pressure (2 Mpa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 3m within 120s 3 The speed of the reaction is increased to 15m at a constant speed 3 And/h, obtaining a ceramic membrane layer, and then sintering at 1375 ℃ for 2.5h, thereby finally preparing the membrane thickness gradient distribution ceramic filter membrane with the membrane porosity of 38 percent, the membrane aperture of 200nm, and the membrane thickness gradually reduced from 55 mu m to 15 mu m along the length direction of the membrane (the direction from the feed end to the discharge end), wherein the pure water flux of the membrane is 2300LMH under the pressure of 0.1 MPa.
Example 2
A layer of paraffin wax of 70 μm (melting point,115 c) film layer and natural cooling, and then the alumina ceramic powder particles (D50 =0.8 μm) for preparing the film layer were heated to 90 c and sprayed on the paraffin film layer using a hot air (85 c) blasting device. The moving speed (0.01 m/s) and the injection pressure (2 Mpa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 6m within 120s 3 H is increased to 12m at a constant speed 3 And/h, obtaining a ceramic membrane layer, and then sintering at 1650 ℃ for 6h, thereby finally preparing the ceramic membrane with the membrane porosity of 32 percent, the membrane aperture of 300nm, and the membrane thickness gradient distribution along the length direction of the membrane (the direction from the feed end to the discharge end) from 50 mu m to 25 mu m, wherein the pure water flux of the ceramic membrane is 2800LMH under the pressure of 0.1 MPa.
Example 3
A 40 μm paraffin (melting point, 60 ℃) film layer was coated on an alumina ceramic membrane support having a pore size of D50=1 μm by a tape casting method and naturally cooled, and then alumina ceramic powder particles (D50 =0.3 μm) for preparing the film layer were heated to 45 ℃ and sprayed on the paraffin film layer by a hot air (45 ℃) blasting device. The moving speed (0.01 m/s) and the injection pressure (2 Mpa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 3m within 120s 3 H is increased to 8m at a constant speed 3 And/h, obtaining a ceramic membrane layer, and then sintering the ceramic membrane layer for 1h at 1120 ℃, thereby finally preparing the membrane thickness gradient distribution ceramic filter membrane with the membrane porosity of 40 percent, the membrane aperture of 80nm, the membrane thickness gradually reduced from 35 mu m to 8 mu m along the length direction of the membrane (the direction from a feed end to a discharge end), and the pure water flux of 2100LMH under the pressure of 0.1 MPa.
Comparative example 1
An alumina ceramic membrane support with a pore diameter of D50=3 μm is coated with a layer of 80 μm paraffin (melting point, 90 ℃) by a tape casting method and is naturally cooled, and then alumina ceramic powder particles (D50 =0.6 μm) for preparing the membrane layer are heated to 65 ℃ and are sprayed on the paraffin membrane layer by a hot air (60 ℃) sand blasting device. The moving speed (0.01 m/s) and the injection pressure (2 Mpa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 3m within 120s 3 The speed of the reaction is increased to 15m at a constant speed 3 And/h, obtaining a ceramic film layer, and then sintering at 1375 ℃ for 2.5h, wherein the film layer is seriously peeled off.
Comparative example 2
A 30 μm paraffin (melting point, 90 ℃) film layer was coated on an alumina ceramic membrane support having a pore diameter of D50=3 μm by a tape casting method and naturally cooled, and then alumina ceramic powder particles (D50 =0.6 μm) for preparing the film layer were heated to 65 ℃ and sprayed on the paraffin film layer by using a hot air (60 ℃) blasting device. The moving speed (0.01 m/s) and the injection pressure (2 Mpa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 3m within 120s 3 H is increased to 15m at uniform speed 3 And/h, obtaining a ceramic membrane layer, and then sintering at 1375 ℃ for 2.5h, wherein the membrane layer has low strength, loose combination and partial position falling off.
Comparative example 3
A 45 μm paraffin (melting point, 90 ℃) film layer was coated on an alumina ceramic film support with a pore diameter D50=3 μm by a tape casting method and naturally cooled, and then alumina ceramic powder particles (D50 =0.6 μm) for preparing the film layer were heated to 65 ℃ and sprayed on the paraffin film layer by a hot air (60 ℃) blasting device. The moving speed (0.01 m/s) and the injection pressure (2 MPa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 2m within 120s 3 H is increased to 15m at uniform speed 3 And/h, obtaining a ceramic film layer, and then sintering at 1375 ℃ for 2.5h, thereby finally preparing the ceramic film with the film porosity of 38 percent, the film aperture of 200nm, the film thickness gradually reduced from 55 mu m to 5 mu m along the length direction of the film (the direction from the feed end to the discharge end), the tail end film layer of the ceramic film is thin, the strength is low, and the pure water flux is 3200LMH under the pressure of 0.1 MPa.
Comparative example 4
A 45 μm paraffin (melting point, 90 ℃) film layer was coated on an alumina ceramic film support with a pore diameter D50=3 μm by a tape casting method and naturally cooled, and then alumina ceramic powder particles (D50 =0.6 μm) for preparing the film layer were heated to 65 ℃ and sprayed on the paraffin film layer by a hot air (60 ℃) blasting device. The moving speed (0.01 m/s) and the injection pressure (2 Mpa) of the sand blasting equipment are fixed, and the sand blasting flow is controlled to be 3m within 120s 3 H is increased to 16m at a constant speed 3 The ceramic membrane layer is obtained and then sintered for 2.5 hours at 1375 ℃, thereby finally preparing the membrane with the porosity of 38 percent and the membrane pore diameter of 200nm along the length direction of the membrane (entering the length direction of the membrane)The direction from the material end to the material discharge end) of the ceramic membrane with gradient distribution, the thickness of the ceramic membrane is gradually reduced from 62 mu m to 15 mu m, the tail end membrane layer is too thick, the membrane resistance is large, the sintering strength is low, and the pure water flux is 1900LMH under the pressure of 0.1 MPa.
A comparison of the products obtained in the examples and comparative examples is shown in the following table:
according to the invention, the position with large thickness of the ceramic membrane layer is used as a feeding end, the filtering resistance is large, the position with small thickness of the ceramic membrane layer is used as a discharging end, and the filtering resistance is small, so that the problems of large pressure of a feeding port, small pressure of a discharging port, uneven membrane flux and membrane pollution and low effective utilization rate of the membrane in cross-flow filtration are solved.
In the preparation method, the paraffin film layer becomes soft due to the blowing of the hot air, and the film layer ceramic powder can be embedded into the paraffin film layer by utilizing the kinetic energy given by the sand blasting equipment and the heat energy carried by the powder and is tightly stacked. The paraffin film layer can also firmly adhere the embedded ceramic particles by utilizing the self viscosity, simultaneously fix the spraying pressure and the moving speed of the sand blasting equipment, and control the sand blasting amount of the ceramic particles on the film surface section by controlling the sand blasting flow rate of the corresponding film surface to be sprayed, thereby depositing the ceramic film layer with the thickness gradient distribution along the length direction of the film on the ceramic film support body.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (2)
1. A preparation method of a ceramic filter membrane with gradient distribution of membrane thickness is characterized by comprising the following steps: the pure water flux of the ceramic filter membrane with the membrane thickness gradient distribution under the pressure of 0.1MPa is 2100-3200LMH, the ceramic filter membrane comprises a ceramic membrane support body and a ceramic membrane layer arranged on the surface of the ceramic membrane support body, the thickness of the ceramic membrane layer is gradually reduced along the direction from a feed end to a discharge end, the thickness is gradually reduced from 35-55 mu m to 8-25 mu m, the porosity of the ceramic membrane layer is 32-40%, and the pore diameter is 80-300nm;
the preparation method comprises the following steps:
(1) Coating a paraffin film layer with the thickness of 40-70 μm on a ceramic membrane support with the aperture D50=1-8 μm, and naturally cooling, wherein the melting point of the paraffin is 60-115 ℃;
(2) Heating ceramic powder particles with D50=0.3-0.8 μm for preparing a ceramic film layer to 80-100 ℃, and then spraying the ceramic powder particles to the paraffin film layer by using a hot air sand blasting device, wherein under the condition of fixed spraying pressure and moving speed, the sand blasting flow of the hot air sand blasting device is uniformly increased from 3-6 m/h to 8-15 m/h in a 120s direction from one end to the other end of the ceramic film support body, the spraying pressure of the hot air sand blasting device is 1.8-2.2MPa, and the moving speed of the hot air sand blasting device is 0.008-0.012m/s;
(3) And (3) sintering the material obtained in the step (2), wherein the sintering temperature is 1100-1700 ℃, and the sintering time is 2-6h, so as to obtain the ceramic filter membrane with the membrane thickness gradient distribution.
2. The method for preparing a membrane thickness gradient distribution ceramic filtration membrane according to claim 1, wherein: the temperature of hot air of the hot air sand blasting device is 45-85 ℃.
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| CN202011054546.7A CN114307688B (en) | 2020-09-29 | 2020-09-29 | Membrane thickness gradient distribution ceramic filtering membrane and preparation method thereof |
| PCT/CN2020/140326 WO2022068110A1 (en) | 2020-09-29 | 2020-12-28 | Ceramic filter membrane with membrane thickness in gradient distribution, and preparation method therefor |
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| CN202011054546.7A CN114307688B (en) | 2020-09-29 | 2020-09-29 | Membrane thickness gradient distribution ceramic filtering membrane and preparation method thereof |
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| WO2022068110A1 (en) | 2022-04-07 |
| CN114307688A (en) | 2022-04-12 |
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