CN112675712A - Preparation method of roll-type ceramic membrane, prepared product and filtration water purifier - Google Patents
Preparation method of roll-type ceramic membrane, prepared product and filtration water purifier Download PDFInfo
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- CN112675712A CN112675712A CN202011457578.1A CN202011457578A CN112675712A CN 112675712 A CN112675712 A CN 112675712A CN 202011457578 A CN202011457578 A CN 202011457578A CN 112675712 A CN112675712 A CN 112675712A
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Abstract
The invention discloses a preparation method of a rolled ceramic membrane, which is characterized in that a flexible flat ceramic membrane with a permeation channel is rolled to form a rolled ceramic membrane support body with every rolling layer at intervals, and then a separation membrane layer is prepared on the outer surface of the rolled ceramic membrane to obtain the rolled ceramic membrane. In addition, the product prepared by the preparation method and the filtration water purifier are also disclosed. The prepared roll-type structure ceramic membrane is based on a flat ceramic membrane structure, greatly improves the membrane area by curling, and realizes the self-support of the ceramic membrane by utilizing the rigidity of a ceramic material, thereby being obviously superior to the organic membrane needing a specific support structure. The water purifier does not need auxiliary energy to provide power, has excellent filtering performance, does not generate waste water in the operation process, and does not influence the natural circulation of tap water.
Description
Technical Field
The invention relates to the technical field of ceramic membrane separation, in particular to a preparation method of a ceramic membrane, a prepared product and a filtration water purifier.
Background
The inorganic ceramic membrane has the advantages of high temperature resistance, solvent resistance, acid and alkali corrosion resistance, high mechanical strength, easy cleaning, regeneration and the like, and has unique technical advantages in the fields of petrochemical industry, food, pharmacy, environmental protection and the like. Currently, common configurations for inorganic membranes are single tubular, multi-channel tubular, flat and disk. Overall, the above configuration results in a relatively small membrane area per unit volume of the inorganic membrane module. The organic membrane with the roll-shaped structure can greatly increase the membrane area in unit volume and reduce the disposable hardware investment of the membrane separation equipment. But it is difficult for the inorganic film to obtain a roll structure like an organic film due to the rigidity of the inorganic material. At present, the prior art also develops an inorganic membrane element with a high membrane area/volume ratio, namely, a hollow fiber inorganic membrane is filled in honeycomb ceramics, so that the membrane area/volume ratio of the inorganic membrane is effectively improved, and simultaneously, the contradiction between the configuration of the hollow fiber inorganic membrane and the filtration mode of the hollow fiber inorganic membrane is effectively solved. However, this configuration of port sealing is relatively complex.
Further, the household water purifier is substantially miniaturized for advanced water treatment, and the main treatment objects are turbidity, chromaticity, odor, organic substances, and the like in tap water. Generally comprises three parts of pre-filtration (rough filtration), adsorption, fine filtration (micro filtration, ultra filtration, reverse osmosis) and the like. Among the composite water purifiers, the composite water purifier based on the membrane technology has excellent water purification performance and particularly has a remarkable effect on removing microorganisms (bacteria, algae and the like). At present, hollow fiber organic membranes are the mainstream, bundled hollow fiber ultrafiltration membranes are prepared into a ultrafiltration core through a casting process, and the filter core consists of an ABS shell, epoxy seal heads at two ends of the shell and the bundled hollow fiber ultrafiltration membranes. The epoxy seal head fills the gap between the hollow fiber ultrafiltration membranes, and isolates the stock solution and the permeate solution. The hollow fiber membrane can not be cleaned, so that the hollow fiber membrane is used as the terminal sterilization of water purification equipment and needs to be replaced for 1 to 2 years generally. Secondly, the water treatment device has the disadvantage that the pressure of the water is lower than the working pressure, so a booster pump is needed, and the power and the pressure are needed. The major disadvantage is that the waste water is much, and about 50% of the waste water is generally filtered.
At present, the adopted ceramic filtering water purifier mainly adopts an inserted ceramic filter element, and a double-control membrane ceramic filter element with the highest precision of 0.1 mu m can completely isolate bacteria outside the filter element, so that secondary pollution can not be generated, the filter element is not afraid of blockage, and the terminal water purifying function is realized. But the disadvantages are that the filter element has short service life, small water yield and large volume, and also needs a booster pump.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a rolled ceramic membrane. The invention also aims to provide a product prepared by the preparation method and a filtration water purifier.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a roll-type ceramic membrane, which comprises the following steps:
(1) preparation of roll type ceramic membrane support
(1-1) extruding and molding the plastic ceramic pug into a rectangular flat ceramic membrane with a permeation channel inside by adopting an extrusion molding method, then placing an elastic spacer on the rectangular flat ceramic membrane, and curling the elastic spacer and the permeation channel together along the direction of the permeation channel to obtain a cylindrical blank with a spiral cross section; wherein, the starting end of the flat ceramic membrane is sealed, and the tail end of the flat ceramic membrane is folded away from the cylindrical outer side to form a water outlet end;
(1-2) drying and shaping the cylindrical blank, removing the elastic spacer, and sintering to obtain the roll-type ceramic membrane support body with intervals between the curled outer surfaces;
(2) preparation of separation membrane layer
And horizontally placing the roll-type ceramic membrane support in the suspension slurry with the water outlet end upward, and preparing a separation membrane layer on the outer surface of the roll-type ceramic membrane support by adopting a dip-coating method to obtain the roll-type ceramic membrane.
Further, the plastic ceramic pug comprises the following raw materials: the plastic ceramic pug comprises ceramic powder with the average particle size of 5-50 mu m, and pore-forming agent, binder, water, lubricant and plasticizer with the dosage of 1-8 wt%, 2-6 wt%, 10-38 wt%, 3-6 wt% and 0.5-1.5 wt% of the ceramic powder respectively; firstly, mixing ceramic powder, a pore-forming agent and a binder in a mixer to form uniform mixed powder; and kneading the mixed powder with water, a lubricant and a plasticizer in a pug kneading machine to obtain pug, and ageing to obtain the plastic ceramic pug.
The suspension slurry comprises the following raw materials: the suspension slurry is composed of ceramic powder with the average particle size of 0.5-1 mu m, and a dispersant, a stabilizer and water with the dosage of 0.5-1.2 wt%, 1-4 wt% and 700-920 wt% of the ceramic powder respectively, and the suspension slurry is obtained by stirring and mixing uniformly.
Further, drying the cylindrical blank body in the step (1-2) at the temperature of 60-90 ℃ for more than 10 hours; sintering at 1300-1650 ℃, and calcining for 2-4 h.
In the scheme, the ceramic powder is Al2O3、ZrO2、TiO2、SiO2SiC, or a combination thereof. The pore-forming agent is starch; the binder is one or the combination of carboxymethyl cellulose, methyl cellulose, polyvinyl alcohol and hydroxypropyl methyl cellulose; the lubricant is glycerol and/or oleic acid; the plasticizer is polyvinyl alcohol. The dispersant is one or the combination of polyacrylic acid, Dolapix series dispersant and polyvinylpyrrolidone, or polyethyleneimine, or the combination of polyethyleneimine and polyvinylpyrrolidone; the stabilizer is one or the combination of polyacrylic acid or polyethyleneimine, polypropylene pyrrolidone and polyvinyl alcohol (polyacrylic acid cannot be used in cooperation with polyethyleneimine).
In the scheme, the elastic spacer is a silicon rubber sheet, a copper sheet or a stainless steel sheet.
The other purpose of the invention is realized by the following technical scheme:
the roll-type ceramic membrane prepared by the preparation method of the roll-type ceramic membrane.
The invention provides a filtering water purifier, which comprises a shell and a filter element; the filter element is the roll-type ceramic membrane; the shell is composed of a cylinder and an end cover with a connecting pipe orifice in the center, and an axial opening is formed in the side face of the cylinder; the filter element, namely the roll-type ceramic membrane, is arranged in the cylinder, and the water outlet end of the filter element extends out of the axial opening of the cylinder; the end caps are sealed at both ends of the cylinder. When the water purifier is used, the connecting pipe orifices at the two ends of the water purifier are connected with a tap water pipe to be respectively used as an inlet and an outlet of water, and the water outlet end of the rolled ceramic membrane extending out of the axial opening of the cylinder is a seepage water outlet. Tap water flows through the filter element, and water filtered and purified by the separation film layer on the outer surface of the roll-type ceramic film enters the permeation channel and is discharged from the permeation water outlet.
The invention has the following beneficial effects:
(1) the ceramic membrane with the roll-type structure is based on a flat ceramic membrane structure, namely, a membrane layer for a separation function is positioned on the outer surface (outer membrane structure), and a higher membrane area/unit volume is obtained by rolling. The outer membrane structure of the flat ceramic membrane is utilized, so that the membrane area is not limited in the pore channel, and the double-sided structure of the flat membrane is added, thereby greatly improving the membrane area.
(2) The present invention utilizes the rigidity of the ceramic material to provide self-support of the ceramic membrane. After drying, shaping and sintering, certain intervals exist between the curled ceramic membrane ring layers to be used as passages of tap water. This spacing does not disappear due to the tap water pressure, enabling self-support, and thus significantly better than organic membranes requiring a specific support structure.
(3) The water filter does not need auxiliary energy to provide power. For ultrafiltration ceramic membranes with membrane pore size of 50nm, the municipal tap water pressure (0.2MPa) is relatively low, but since the rolled ceramic membranes proposed by the present invention have a very high membrane area per unit volume, still a large permeate flux can be obtained. While for 200nm microfiltration membranes, municipal tap water pressure is the optimum pressure to achieve maximum permeate flux. Therefore, the roll type ceramic membrane household water purifier can not depend on external power.
(4) The water purifier does not generate waste water in the running process. The water purifier adopts a mode of parallelly connecting tap water pipes to lead tap water to pass through the water purifier and obtain osmotic pressure from the tap water. Tap water flows in from the inlet and out from the outlet of the water filtering purifier, and a water storage tank is not needed, so that the natural circulation of the tap water is not influenced. The water filtered and purified by the ceramic membrane is collected by the internal permeation channel of the ceramic membrane and flows out from the water outlet end (permeation water outlet) at the lateral opening of the water purifier for use.
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 a flat ceramic diaphragm according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing the curling of a flat ceramic diaphragm and an elastic spacer according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a second filtration water purifier according to an embodiment of the present invention.
In the figure: the filter comprises a flat ceramic membrane 1, a permeation channel 1a, a water outlet end 1b, an elastic spacer 2, a filter element 3, a cylinder 4, an axial opening 4a, an end cover 5 and a connecting pipe orifice 5a
Detailed Description
The first embodiment is as follows:
the preparation method of the roll-type ceramic membrane comprises the following steps:
(1) preparation of roll type ceramic membrane support
(1-1) mixing 100kg of alumina powder (with the average particle size of 40 mu m), 8kg of starch and 5kg of hydroxypropyl methyl cellulose in a mixer to obtain uniform mixed powder; kneading the mixed powder with 18kg of water, 2kg of glycerol and 1kg of polyvinyl alcohol in a pug kneading machine to obtain mud, and ageing for 1 week to obtain plastic ceramic pug; extruding and molding the plastic ceramic mud into a rectangular flat ceramic membrane 1 (length is 55mm, width is 12.5mm and thickness is 3mm) with permeation channels 1a (length is 3mm, width is 1mm and the permeation channels are spaced by 1mm) as shown in figure 1 by adopting an extrusion molding method, and flattening a port at one end by adopting a straight ruler to finish sealing the port; then placing a silicon rubber sheet with the thickness of 2mm on the water outlet pipe as an elastic spacer 2, curling the water outlet pipe and the water outlet pipe together along the direction of a permeation channel by taking one sealed end as an initial end to obtain a cylindrical blank with a spiral cross section, and folding the curled tail end away from the cylindrical outer side to form a water outlet end 1b (see figure 2);
(1-2) drying the cylindrical blank in a constant-temperature constant-humidity drying box (at the temperature of 80 ℃ and the humidity of 90%) for 12h for shaping, removing silicon rubber sheets, and calcining at 1650 ℃ for 4h to obtain a rolled ceramic membrane support body with the average pore diameter of 1-4 mu m and intervals between the outer surfaces of each roll;
(2) preparation of separation membrane layer
Dissolving 5g of Dolapix CE-64 in 9kg of water, adding 1kg of alumina powder with the average particle size of 1 mu m, adding 35g of polyvinyl alcohol 1750 (prepared by polyvinyl alcohol and added into a solution with the concentration of 10 wt%), and mixing together under the condition of vigorous stirring to obtain suspension slurry; and horizontally placing the rolled ceramic membrane support in the suspension slurry with the water outlet end 1b upward (to prevent the suspension slurry from overflowing to the permeation channel side) for immersing for 1min, taking out, drying at room temperature, and calcining at 1450 ℃ for 3h to obtain a separation membrane layer with the average pore diameter of 0.2 mu m on the outer surface of the rolled ceramic membrane support so as to obtain the rolled ceramic membrane.
Example two:
fig. 3 shows an embodiment of a filtration water purifier of the present invention, which includes a housing and a filter element 3; wherein the filter element 3 is the roll-type ceramic membrane prepared in the first embodiment.
As shown in fig. 3, the housing is composed of a cylinder 4 and an end cap 5 having a connecting nozzle 5a at the center, and an axial opening 4a is provided in the side surface of the cylinder 4. The filter element 3, i.e. the roll-up ceramic membrane, is arranged in the cylinder 4, and the water outlet end 1b thereof extends out of the axial opening 4a of the cylinder. End caps 5 are sealed at both ends of the cylinder 4. When the filtration water purifier is used, the connecting pipe orifices 5a at the two ends of the filtration water purifier are connected with the tap water pipe to be respectively used as the water inlet and the water outlet, and the water outlet end 1b of the rolled ceramic membrane extending out of the axial opening 4a of the cylinder is the permeation water outlet. Tap water flows through the filter element 3, and water filtered and purified by the separation membrane layer on the outer surface of the roll-type ceramic membrane enters the permeation channel 1a and is discharged from the permeation water outlet.
The embodiment filters water purifier mainly filters impurities such as iron rust, silt, macromolecular particles that exist in the running water, does not influence the mineral substance in aquatic.
Example three:
the present embodiment is a method for preparing a rolled ceramic film, which is different from the first embodiment in that:
in the step (2) of preparing the separation membrane layer:
1. dissolving 10g of Dolapix CE-64 in 9kg of water, adding 1kg of alumina powder with the average particle size of 0.2 mu m, adding 30g of polyvinyl alcohol 1750 (prepared by adding 10 wt% of polyvinyl alcohol), and mixing together under the condition of vigorous stirring to obtain suspension slurry.
2. And drying the roll-type ceramic membrane support body dipped with the suspension slurry, and calcining at 1350 ℃ for 2h to obtain a separation membrane layer with the average pore diameter of 50nm on the outer surface of the roll-type ceramic membrane support body, thereby obtaining the roll-type ceramic membrane.
Example four:
the difference between the filtration water purifier of the embodiment and the second embodiment is that: mainly filters organic matters, colloid, large suspended matters, particles, bacteria and the like in tap water, and does not influence the mineral matters in the water.
Claims (10)
1. The preparation method of the roll-type ceramic membrane is characterized by comprising the following steps of:
(1) preparation of roll type ceramic membrane support
(1-1) extruding and molding the plastic ceramic pug into a rectangular flat ceramic membrane (1) with a permeation channel (1a) inside by adopting an extrusion molding method, then placing an elastic spacer (2) on the rectangular flat ceramic membrane, and curling the elastic spacer and the elastic spacer together along the direction of the permeation channel to obtain a cylindrical blank with a spiral cross section; wherein, the starting end of the flat ceramic membrane (1) is sealed, and the tail end of the flat ceramic membrane (1) is folded away from the cylindrical outer side to form a water outlet end (1 b);
(1-2) drying and shaping the cylindrical blank, removing the elastic spacer (2), and sintering to obtain the rolled ceramic membrane support body with intervals among the curled outer surfaces;
(2) preparation of separation membrane layer
And (3) horizontally placing the roll-type ceramic membrane support body in the suspension slurry with the water outlet end (1b) upward, and preparing a separation membrane layer on the outer surface of the roll-type ceramic membrane support body by adopting a dip-coating method to obtain the roll-type ceramic membrane.
2. The preparation method of roll-type ceramic membrane according to claim 1, characterized in that the plastic ceramic pug comprises the following raw materials: the plastic ceramic pug comprises ceramic powder with the average particle size of 5-50 mu m, and pore-forming agent, binder, water, lubricant and plasticizer with the dosage of 1-8 wt%, 2-6 wt%, 10-38 wt%, 3-6 wt% and 0.5-1.5 wt% of the ceramic powder respectively; firstly, mixing ceramic powder, a pore-forming agent and a binder in a mixer to form uniform mixed powder; and kneading the mixed powder with water, a lubricant and a plasticizer in a pug kneading machine to obtain pug, and ageing to obtain the plastic ceramic pug.
3. The method for preparing roll-type ceramic membrane according to claim 1, wherein the suspension slurry is prepared by the following raw materials: the suspension slurry is composed of ceramic powder with the average particle size of 0.5-1 mu m, and a dispersant, a stabilizer and water with the dosage of 0.5-1.2 wt%, 1-4 wt% and 700-920 wt% of the ceramic powder respectively, and the suspension slurry is obtained by stirring and mixing uniformly.
4. The method for preparing roll-type ceramic membrane according to claim 1, characterized in that: drying the cylindrical blank body in the step (1-2) at the temperature of 60-90 ℃ for more than 10 h; sintering at 1300-1650 ℃, and calcining for 2-4 h.
5. The method for preparing rolled ceramic membrane according to claim 2 or 3, characterized in that: the ceramic powder is Al2O3、ZrO2、TiO2、SiO2SiC, or a combination thereof.
6. The method for preparing roll-type ceramic membrane according to claim 2, characterized in that: the pore-forming agent is starch; the binder is one or the combination of carboxymethyl cellulose, methyl cellulose, polyvinyl alcohol and hydroxypropyl methyl cellulose; the lubricant is glycerol and/or oleic acid; the plasticizer is polyvinyl alcohol.
7. The method for preparing rolled ceramic membrane according to claim 3, characterized in that: the dispersant is one or the combination of polyacrylic acid, Dolapix series dispersant and polyvinylpyrrolidone, or polyethyleneimine, or the combination of polyethyleneimine and polyvinylpyrrolidone; the stabilizer is one or the combination of polyacrylic acid or polyethyleneimine, polypropylene pyrrolidone and polyvinyl alcohol.
8. The method for preparing roll-type ceramic membrane according to claim 1, characterized in that: the elastic spacer can be a silicon rubber sheet, a copper sheet or a stainless steel sheet.
9. Roll-up ceramic membrane produced by the process for the production of a roll-up ceramic membrane according to any one of claims 1 to 8.
10. The utility model provides a filtration water purifier, includes casing and filter core (3), its characterized in that: the filter element (3) is the rolled ceramic membrane according to claim 9; the shell is composed of a cylinder (4) and an end cover (5) with a connecting pipe orifice (5a) in the center, and an axial opening (4a) is formed in the side surface of the cylinder (4); the filter element (3), namely the roll-type ceramic membrane, is arranged in the cylinder (4), and the water outlet end (1b) of the filter element extends out of the axial opening (4a) of the cylinder; the end covers 5 are sealed at two ends of the cylinder (4).
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