CN110368820B - Spraying, slurry pouring and film coating device and preparation method of flat plate type ceramic ultrafiltration membrane - Google Patents
Spraying, slurry pouring and film coating device and preparation method of flat plate type ceramic ultrafiltration membrane Download PDFInfo
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- CN110368820B CN110368820B CN201910737100.5A CN201910737100A CN110368820B CN 110368820 B CN110368820 B CN 110368820B CN 201910737100 A CN201910737100 A CN 201910737100A CN 110368820 B CN110368820 B CN 110368820B
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- 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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D69/06—Flat membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
Abstract
The invention discloses a spraying, slurry-sprinkling and film-coating device, which comprises an automatic spraying device and an automatic slurry-sprinkling device; the automatic spraying device comprises a moving track, a clamp, and a support body dust removing device and a spraying mechanism which are sequentially arranged according to the conveying direction; the clamps are movably arranged on the movable track at intervals; the support body dust removing equipment and the spraying mechanism are positioned on two sides of the moving track; the automatic slurry spraying device comprises a conveyor belt, a supporting piece, a slurry box, a valve, a flowmeter and overflow equipment; the supporting pieces are movably arranged on the conveying belt at intervals; the slurry box and the overflow equipment are positioned above one end of the conveyor belt; the outlet of the slurry box is communicated to the overflow equipment through a valve and a flowmeter. In addition, a preparation method of the flat plate type ceramic ultrafiltration membrane based on the device is also disclosed. The invention obviously improves the production efficiency, and adopts the process of spraying first and then pouring slurry, thereby realizing the purpose of preparing the high-performance flat ceramic membrane with high efficiency.
Description
Technical Field
The invention relates to the technical field of membrane separation, in particular to a film coating device and a preparation method of a flat plate type ceramic ultrafiltration membrane.
Background
Membrane technology has been studied as a 21 st century high technology in developed countries such as europe, the united states, japan, and the like as a high-efficiency, green separation technology. With the continuous development of membrane technology, flat ceramic membranes are increasingly used in the fields of petrochemical industry, sewage treatment and the like due to the advantages of simple structure, small pressure between membranes, low cost, small occupied area of membrane modules and the like.
The flat ceramic membrane is mainly characterized in that the wall of the support body is thin, and the separation membrane layer is positioned on the outer surface of the support body. At present, the preparation of the membrane layer of the flat plate type ceramic ultrafiltration membrane mainly adopts a slurry dipping method and a spraying method.
When the flat-plate ceramic ultrafiltration membrane layer is prepared by adopting a slurry dipping method, at least two times of coating and two times of firing are needed mainly based on the capillary colloidal filtration and the film coating mechanism, the production cost is higher, and the defects that the membrane layer thickness is not uniform, a separation membrane layer is easy to leak, partial holes are blocked, the pure water flux is lower, the pressure between membranes is larger and the like easily occur because the wall of a support body is relatively thin exist. In addition, due to the unique configuration of the flat ceramic membrane (the wall is thin and the middle is connected by the rib part), particles with the particle size smaller than the pore size of the support in the coating slurry of the separation layer are easy to leak into the support to block the pore channel, and the defects of uneven thickness of the rib part of the support and the non-rib part of the membrane layer are generated at the same time.
When the flat ceramic ultrafiltration membrane layer is prepared by a spraying method, the method is mainly based on the principle of layer-by-layer accumulation of powder particles in ceramic membrane slurry, and has the main problems of uneven surface and poor coating effect. Therefore, the prior art has developed a method of atomizing the spray liquid into ultrafine droplets by means of an ultrasonic atomizing device and an auxiliary air flow, and then the ultrafine droplets are stacked layer by layer to form a film layer. In the methods, multiple layers of spraying are often needed, the defects of unsmooth film surface, bubble generation, macropore generation and the like are easily caused, the process is complex, the energy consumption is high, the automation degree is low, and great difficulty is brought to high-efficiency film coating and high-performance preparation of the flat ceramic film.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a slurry spraying and coating device, so that a flat ceramic membrane support body can be coated in a coating mode of automatically spraying and then automatically spraying, the preparation process is simplified, and the production efficiency is improved. The invention also aims to provide a preparation method of the flat plate type ceramic ultrafiltration membrane based on the device, which comprises the steps of firstly preparing an intermediate isolation layer by adopting a spraying method, then preparing a separation membrane layer by adopting a slurry pouring method, and directly preparing a ceramic membrane with smaller pore diameter on a large-pore support body through one-time drying and sintering, thereby realizing the preparation of a high-performance flat plate ceramic membrane with high efficiency.
The purpose of the invention is realized by the following technical scheme:
the invention provides a spraying, slurry-sprinkling and film-coating device, which comprises an automatic spraying device and an automatic slurry-sprinkling device;
the automatic spraying device comprises a moving track, a clamp with a clamping groove, and a support body dust removing device and a spraying mechanism which are sequentially arranged in the conveying direction; the fixture is movably arranged on the movable track at intervals, and pore ports at two ends of the support body are clamped in clamping grooves of the fixture; the support body dust removing equipment is positioned on two sides of the moving track; the spraying mechanism comprises a spraying kettle, a compressor, an atomizing nozzle bracket, an atomizing nozzle, a residual slurry collecting baffle and a residual slurry collecting tank; the residual slurry collecting baffle plates are in an inwards concave arc shape and are symmetrically arranged on two sides of the moving track; the atomizing nozzle support is positioned in the middle of the residual slurry baffle area and symmetrically arranged on two sides of the moving track; the atomizing nozzles are arranged on the atomizing nozzle bracket in the vertical direction and are connected with the spray can and the compressor; the residual slurry collecting tank is positioned below the moving track and corresponds to the residual slurry collecting baffle;
the automatic slurry spraying device comprises a conveyor belt, a supporting piece with a boss, a slurry box, a valve, a flowmeter and overflow equipment; the supporting pieces are movably arranged on the conveying belt at intervals; the slurry box and the overflow equipment are positioned above one end of the conveyor belt; and the outlet of the slurry box is communicated to overflow equipment through a valve and a flowmeter.
The other purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a flat plate type ceramic ultrafiltration membrane based on the device, which comprises the following steps:
(1) preparation of ceramic suspension slurry
According to the raw material composition, 15-33 wt% of ceramic powder with the particle size D50 of 0.1-1 mu m, 1-3 wt% of polyvinyl alcohol, 0.1-0.5 wt% of dispersing agent and 65-83 wt% of deionized water, firstly, uniformly mixing the deionized water and the dispersing agent, then adding the ceramic powder for ultrasonic dispersion, then adding the polyvinyl alcohol, stirring and mixing to obtain a mixed solution; ball-milling and uniformly mixing the mixed solution to obtain ceramic suspension slurry;
(2) preparation of isolating layer by spraying method
Based on the automatic spraying device, the ceramic suspension slurry is filled into a spraying pot, the speed of the moving track is 0.05-0.2 m/s, and the clamp carries the support body to move along with the moving track; spraying the ceramic suspension slurry on a flat ceramic membrane support through the atomizing nozzle at the pressure of 0.1-0.25 MPa and the flow rate of 150-300 mL/min to form an isolation layer, so as to obtain the flat ceramic membrane support containing the isolation layer;
(3) preparation of separation film layer by slurry spraying method
Based on the automatic slurry spraying device, the speed of the conveyor belt is 0.1-0.25 m/s, and the flat ceramic membrane support body containing the isolation layer is flatly placed on the support and runs along with the conveyor belt; loading the ceramic suspension slurry into a slurry box, opening a valve, enabling the ceramic suspension slurry to flow through overflow equipment and then flow out, and carrying out single-side slurry spraying on the surface of the flat ceramic membrane support body containing the isolation layer at a flow rate of 200-400 mL/min; inverting the flat ceramic membrane support body containing the isolation layer, and then performing single-side slurry spraying again to obtain the flat ceramic membrane support body containing the separation membrane layer and the isolation layer;
(4) preparation of flat plate type ceramic ultrafiltration membrane
And drying the flat ceramic membrane support body containing the separation membrane layer and the isolation layer, and calcining to obtain the flat ceramic ultrafiltration membrane.
Furthermore, the ultrasonic dispersion time in the step (1) is 30-50 min, the stirring and mixing time is 30-60 min, and the ball milling and mixing time is 90-180 min.
Furthermore, the solid content of the ceramic suspension slurry is 15-35 wt%, and the viscosity is 30-60 Pa.s.
Furthermore, the thickness of the isolation layer is 15-25 μm, and the thickness of the separation film layer is 10-20 μm.
Furthermore, in the step (4), the drying temperature is 40-100 ℃, and the calcining temperature is 1200-1350 ℃.
The invention has the following beneficial effects:
(1) the invention utilizes the automatic spraying and slurry pouring device and is provided with the clamp and the supporting piece at the same time, and can realize the bidirectional sealing treatment of the section of the supporting body, thereby effectively preventing slurry from entering the inner surface of the supporting body, ensuring the high porosity and the high permeation flux of the flat ceramic membrane, greatly saving the coating time and obviously improving the production efficiency.
(2) According to the invention, the process of spraying and then pouring slurry is adopted, the isolating layer obtained by spraying can effectively isolate the defects of macropores and the like of the support body, and the membrane layer obtained by pouring slurry can further fill and level up and eliminate the defects of uneven surface, bubbles and the like of the isolating layer, so that the ceramic membrane with smaller pore diameter is directly prepared on the support body with large pore diameter, and the problems of unsmooth membrane surface, easy leakage of the membrane layer, uneven membrane thickness, lower flux, macropore defects and the like of the ceramic ultrafiltration membrane prepared by the spraying method in the prior art are effectively solved.
(3) According to the invention, the ceramic membrane product can be prepared by one-time drying and sintering, so that the problems of complex preparation process, more sintering times and higher energy consumption of the conventional flat plate ceramic ultrafiltration membrane are effectively solved; the residual slurry baffle is combined with the spraying process, so that the cyclic utilization of the coating slurry is realized, and the preparation cost of the flat ceramic membrane is greatly saved.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 is a schematic structural diagram of an automatic coating apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic view of a fixture in the automatic spray coating apparatus of FIG. 1;
FIG. 3 is a schematic view showing the connection between the support and the jig in the automatic spray coating apparatus shown in FIG. 1;
FIG. 4 is a schematic view of a residual slurry collecting baffle in the automatic spray coating apparatus shown in FIG. 2;
FIG. 5 is a schematic view of the structure of an automatic slurry spraying device in the embodiment of the present invention;
FIG. 6 is a schematic view of the connection between the support and the flat ceramic membrane support with the isolation layer in the automatic slurry spraying apparatus shown in FIG. 5;
FIG. 7 is a flow chart of a manufacturing process for an embodiment of the present invention;
FIG. 8 is a surface SEM photograph of a separation membrane layer produced by spray coating according to an embodiment of the present invention;
FIG. 9 is a SEM photograph showing the cross section of a flat plate type ceramic ultrafiltration membrane according to an example of the present invention.
In the figure: moving track 1, anchor clamps 2, draw-in groove 2a, supporter dust collecting equipment 3, supporter 4, atomizing nozzle support 5, atomizing nozzle 6, surplus thick liquid collecting baffle 7, surplus thick liquid collecting vat 8, conveyer belt 9, supporting part 10, boss 10a, thick liquid case 11, valve 12, flowmeter 13, overflow apparatus 14
Detailed Description
Fig. 1 to 9 show an embodiment of a spray slurry coating device and a method for manufacturing a flat plate type ceramic ultrafiltration membrane according to the present invention.
The spraying, slurry pouring and film coating device comprises an automatic spraying device and an automatic slurry pouring device.
As shown in fig. 1, the automatic spraying device includes a moving rail 1, a jig 2 (see fig. 2) having a clamping groove 2a, and a support body dust removing device 3 and a spraying mechanism which are sequentially arranged in a conveying direction; the clamps 2 are movably arranged on the moving track 1 at intervals, and pore channel ports at two ends of the support body 4 are clamped in clamping grooves 2a of the clamps 2 (see fig. 3); the support body dust removing equipment 3 is positioned on two sides of the moving track 1; the spraying mechanism comprises a spraying kettle, a compressor, an atomizing nozzle bracket 5, an atomizing nozzle 6, a residual slurry collecting baffle 7 and a residual slurry collecting tank 8; the residual pulp collecting baffle 7 is in an inward concave arc shape (see figure 4) and is symmetrically arranged at two sides of the moving track 1; the atomizing nozzle supports 5 are positioned in the middle of the residual slurry baffle area and symmetrically arranged on two sides of the moving track 1; the atomizing nozzles 6 are arranged on the atomizing nozzle bracket 5 in the vertical direction and are connected with the spray can and the compressor; the residual slurry collecting tank 8 is positioned below the movable track 1 and corresponds to the residual slurry collecting baffle 7.
As shown in fig. 5, the automatic slurry pouring device comprises a conveyor belt 9, a support 10 with a boss 10a, a slurry tank 11, a valve 12, a flowmeter 13 and an overflow device 14; the supporting members 10 are movably arranged on the conveyor belt 9 at intervals; the slurry box 11 and the overflow device 14 are positioned above one end of the conveyor belt 9; the outlet of the slurry tank 11 is connected to an overflow device 14 via a valve 12 and a flow meter 13.
In this example, the method for preparing a flat ceramic ultrafiltration membrane based on the above apparatus, using a flat ceramic membrane support (length 500mm × width 100mm × thickness 3mm) with an average pore size of 4 μm as a substrate, as shown in fig. 7, comprises the following steps:
(1) preparation of ceramic suspension slurry
According to the technical scheme, the method comprises the following steps of (1) uniformly mixing 24 wt% of alumina powder (D50 is 0.6 mu m), 1.8 wt% of polyvinyl alcohol, 1.8 wt% of dispersant Dolapix CE-640.2 wt% and 74 wt% of deionized water according to raw material composition, adding the alumina powder, performing ultrasonic dispersion for 30min, adding the polyvinyl alcohol, stirring and mixing for 30min to obtain a mixed solution; pouring the mixed solution into a ball milling tank for ball milling for 120min (the rotating speed is 200r/min), thus obtaining stable ceramic suspension slurry with the solid content of 24 wt% and the viscosity of 35 Pa.s;
(2) preparation of isolating layer by spraying method
Filling the ceramic suspension slurry into a sprinkling can; the automatic spraying device shown in fig. 1 is adopted to clamp the two ends of the support body 4 in the clamping grooves 2a of the clamp 2 (see fig. 3), so that the pore channel ports of the support body 4 are closed in two directions; opening the moving track 1 (the speed is 0.1m/s), enabling the clamp 2 to carry the support 4 to move along with the moving track 1, removing dust on the surface of the support by compressed air through the support dust removing equipment 3, and then continuously moving to the spraying mechanism, wherein in the operation process, the ceramic suspension slurry is sprayed on the surface of the support 4 through the atomizing nozzle 6 at the pressure of 0.15MPa and the flow rate of 150mL/min to form an isolation layer, so that the flat ceramic membrane support containing the isolation layer is obtained; the sprayed slurry flows into a residual slurry collecting tank 8 through a residual slurry collecting baffle 7;
(3) preparation of separation film layer by slurry spraying method
Adopting an automatic slurry spraying device as shown in fig. 5, flatly placing and erecting the flat ceramic membrane support body containing the isolating layer between two supporting pieces 10, and enabling the end head to be abutted against the side surface of a boss 10a (see fig. 6), so that the pore channel port of the support body is closed in two directions; starting the conveyor belt 9 (with the speed of 0.12m/s), and enabling the support 10 to carry the flat ceramic membrane support body containing the isolation layer to run along with the conveyor belt; loading the ceramic suspension slurry into a slurry box 11, opening a valve 12, overflowing and flowing the ceramic suspension slurry after the ceramic suspension slurry flows over an overflow device 14, and performing single-side slurry spraying on the surface of the flat ceramic membrane support containing the isolation layer at a flow rate of 200 mL/min; then, turning over the other side by a manipulator, and spraying slurry on the single side of the other side again to obtain a flat ceramic membrane support body containing a separation membrane layer and an isolation layer;
(4) preparation of flat plate type ceramic ultrafiltration membrane
Drying the flat ceramic membrane support containing the separation membrane layer and the isolation layer at the temperature of 40 ℃ and the humidity of 70% for 5 hours, and then drying at the temperature of 90 ℃ and the humidity of 40% for 5 hours; then calcining at a heating rate of 2.5 ℃/min, and keeping the temperature at 1250 ℃ for 0.5h to obtain a uniform film layer with an average pore diameter of 65nm and a pure water flux of 890L/m2A flat plate ceramic ultrafiltration membrane at bar h.
The flat plate type ceramic ultrafiltration membrane prepared in this example had a separation layer thickness of 20 μm and a separation membrane layer thickness of 18 μm. As shown in fig. 8 and 9, the surface of the membrane layer was smooth and free of defects, the boundaries between the support, the separator layer and the separation membrane layer were clear, and the separator layer did not leak into the interior of the support.
Claims (6)
1. The spraying, slurry spraying and film coating device is characterized in that: comprises an automatic spraying device and an automatic slurry spraying device;
the automatic spraying device comprises a moving track (1), a clamp (2) with a clamping groove (2a), and a support body dust removing device (3) and a spraying mechanism which are sequentially arranged in the conveying direction; the fixture (2) is movably arranged on the movable track (1) at intervals, and pore channel ports at two ends of the support body (4) are clamped in the clamping groove (2a) of the fixture (2); the support body dust removing equipment (3) is positioned on two sides of the moving track (1); the spraying mechanism comprises a spraying kettle, a compressor, an atomizing nozzle support (5), an atomizing nozzle (6), a residual slurry collecting baffle (7) and a residual slurry collecting tank (8); the residual pulp collecting baffle plates (7) are in an inwards concave arc shape and are symmetrically arranged on two sides of the moving track (1); the atomizing nozzle support (5) is positioned in the middle of the residual slurry baffle area and symmetrically arranged on two sides of the moving track (1); the atomizing nozzles (6) are arranged on the atomizing nozzle bracket (5) in the vertical direction and are connected with the spray can and the compressor; the residual slurry collecting tank (8) is positioned below the moving track (1) and corresponds to the residual slurry collecting baffle (7);
the automatic slurry spraying device comprises a conveyor belt (9), a supporting piece (10) with a boss (10a), a slurry box (11), a valve (12), a flowmeter (13) and overflow equipment (14); the supporting pieces (10) are arranged on the conveyor belt (9) at intervals in a movable manner, the supporting body processed by the automatic spraying device is flatly placed and erected between the two supporting pieces (10), and the end of the supporting body abuts against the side face of the boss (10a), so that the pore channel port of the supporting body is closed in a two-way manner; the slurry box (11) and the overflow equipment (14) are positioned above one end of the conveyor belt (9); the outlet of the slurry tank (11) is communicated with an overflow device (14) through a valve (12) and a flowmeter (13).
2. A method for preparing a flat plate type ceramic ultrafiltration membrane is characterized by comprising the following steps:
(1) preparation of ceramic suspension slurry
According to the raw material composition, 15-33 wt% of ceramic powder with the particle size D50 of 0.1-1 mu m, 1-3 wt% of polyvinyl alcohol, 0.1-0.5 wt% of dispersing agent and 65-83 wt% of deionized water, firstly, uniformly mixing the deionized water and the dispersing agent, then adding the ceramic powder for ultrasonic dispersion, then adding the polyvinyl alcohol, stirring and mixing to obtain a mixed solution; ball-milling and uniformly mixing the mixed solution to obtain ceramic suspension slurry;
(2) preparation of isolating layer by spraying method
The automatic spraying device in the spraying, slurry-pouring and film-coating device according to claim 1 is used for loading the ceramic suspension slurry into a spraying pot, the speed of the moving track (1) is 0.05-0.2 m/s, and the clamp (2) carries the support body (4) to move along with the moving track (1); spraying the ceramic suspension slurry on a flat ceramic membrane support through the atomizing nozzle (6) at the pressure of 0.1-0.25 MPa and the flow rate of 150-300 mL/min to form an isolation layer, so as to obtain the flat ceramic membrane support containing the isolation layer;
(3) preparation of separation film layer by slurry spraying method
The automatic slurry pouring device of the spray slurry pouring and coating device according to claim 1, wherein the speed of the conveyor belt (9) is 0.1-0.25 m/s, the flat ceramic membrane support containing the isolation layer is flatly placed on the support (10) and runs along with the conveyor belt (9); loading the ceramic suspension slurry into a slurry box (11), opening a valve (12), enabling the ceramic suspension slurry to flow over an overflow device (14) and then flow down, and performing single-side slurry spraying on the surface of the flat ceramic membrane support body containing the isolation layer at a flow rate of 200-400 mL/min; inverting the flat ceramic membrane support body containing the isolation layer, and then performing single-side slurry spraying again to obtain the flat ceramic membrane support body containing the separation membrane layer and the isolation layer;
(4) preparation of flat plate type ceramic ultrafiltration membrane
And drying the flat ceramic membrane support body containing the separation membrane layer and the isolation layer, and calcining to obtain the flat ceramic ultrafiltration membrane.
3. The method for producing a flat-plate type ceramic ultrafiltration membrane according to claim 2, wherein: the ultrasonic dispersion time in the step (1) is 30-50 min, the stirring and mixing time is 30-60 min, and the ball milling and mixing time is 90-180 min.
4. The method for producing a flat-plate type ceramic ultrafiltration membrane according to claim 2, wherein: the solid content of the ceramic suspension slurry is 15-35 wt%, and the viscosity is 30-60 Pa.s.
5. The method for producing a flat-plate type ceramic ultrafiltration membrane according to claim 2, wherein: the thickness of the isolation layer is 15-25 mu m, and the thickness of the separation film layer is 10-20 mu m.
6. The method for producing a flat-plate type ceramic ultrafiltration membrane according to claim 2, wherein: in the step (4), the drying temperature is 40-100 ℃, and the calcining temperature is 1200-1350 ℃.
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