CN102614782A - Ceramic filter film of rare-earth modified attapulgite with nano coating and preparation method thereof - Google Patents
Ceramic filter film of rare-earth modified attapulgite with nano coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramic filter film of rare-earth modified attapulgite with a nano coating, which comprises a ceramic supporting body and separation film, wherein the ceramic supporting body is plate-type porous ceramic sintered by modifier added with rate-earth oxide in attapulgite clay and intensifier, the ceramic supporting body has the characteristics of high porosity, uniform pore diameter, high strength, light weight and the like; the separation film is a nano decoration coating, and has outstanding hydrophilicity and lipophobicity. The coating film liquid is produced by nano attapulgite mixing with nano rare-earth oxide and relevant additive dispersing in water, coated on the ceramic supporting body surface via a soak-lifting method, and is sintered at high temperature to form porous separation film with nano surface characteristics; the ceramic filter film can be made into a hollow cavity-type structure, a plurality of combined revolving film components are used in rotary manner, more efficient initiative cross-flow operation can be realized, the film surface is self-cleaned by filter liquid brushing in the revolving process, and the blockage and pollution of the film can be greatly delayed.
Description
Technical field
The present invention relates to film and separate and water-treatment technology field, specially refer to a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane and preparation method thereof.
Background technology
Membrane technology has received unprecedented great attention at present in the world, and the film industry is described as the huge rising industry of development potentiality.Membrane technology as many subject crossing such as material science and process engineering combine, interpenetrate and produce has become the common technology of promotion China in environmental protection, the energy, Chemical Engineering and bioengineering four big pillar industries development.
Membrane material is the core of membrane technology, and the membrane material that is applied at industrial circle at present includes organic polymer membrane material and inorganic material film two big classes.Compare with organic polymer films; High temperature resistant, advantages such as chemical stability good, mechanical strength is high, anti-microbe ability is strong, long service life that inoranic membrane has; Thereby closely during the last ten years inoranic membrane particularly the ceramic membrane technical development is rapid, become the focus of the research of domestic and international membrane technology and application and development.
That the type of ceramic membrane comprises is flat, tubular type, multi-channel type etc.Wherein, flat sheet membrane is mainly used in laboratory or industry monolithic filtration on a small scale; The single channel tubular membrane is low, easy to break broken because of intensity, and its application receives limit value; The ceramic membrane of commodity production at present is mostly with α-A1
2O
3Be feedstock production, be mainly multichannel tubular type film, be made generally in 7,19 and 37 passages, with the mechanical strength of raising tubular membrane and the membrane area in the unit volume.Tubular membrane adopts the cross-flow filtration mode to move usually, helps eliminating film surface concentration polarization and decelerating membrane pollution, and its shortcoming is that its film loading density is far below hollow-fibre membrane, rolled film and plate and frame film.For overcoming the effect of boundary layer that filtrate flows produces in the passage, often need therefore cause energy consumption to increase than higher feeding speed, especially be not suitable for the isolated by filtration of high-viscosity material.
A kind of rotary membrane separation device is invented (ZL 200910224681.9); Wherein organic flat sheet membrane is made into rotary disk type membrane assembly rotating operation in filtrating; This active cross-flow filtration operation had both helped eliminating concentration polarization and decelerating membrane pollution; Can overcome the energy consumption problems of too that aeration washes away or high-speed feeding cycle produces again, and the film surface clean is convenient.Though what the present invention was directed against is organic flat sheet membrane, also good prospect is provided simultaneously for the use of planar ceramic membrane.
Attapulgite (being called for short ATP) belongs to sepiolite group, is a kind of hydrous magnesium aluminosilicate with filamentary structure, and the theoretical chemistry composition is: SiO
256.96%, (Fe) O 23.83%, H for Mg, Al
2O 19.21%.China's attapulgite reserves are abundant, and are cheap, and exploitation and process energy consumption are low, and environmental pollution is light.And the technology of from attapulgite, extracting the natural nano attapulgite is comparative maturity also.Disclosing a kind of production method of attapulgite ceramic size among the ZL201010562427.2, is that raw material is fired light ceramics with the attapulgite clay mineral, and a new way is opened up in the development and use that can be attapulgite.But concavo-convex excellent pottery has shortcomings such as intensity is low, poor stability, is not suitable for directly applying to the flat ceramic supporting body of making.Rare earth element is used as ceramic modified dose and reinforcing agent because its internal layer 4f electron number from 0 to 14 is filled formed special configuration one by one, can significantly improve the compression strength of ceramic material.
In the separation process of ceramic filtration membrane, membrane resistance mainly concentrates on the teleblem.With nanocrystalline ceramic membrane is carried out the coating modifying modification, particularly use nano-TiO
2, ZrO
2As modifier, can effectively improve the hydrophily and the characteristic such as charged of film surface hydroxyl Deng metal oxide, and cause the remarkable increase of water flux thus.The natural nano attapulgite is cheap and easy to get, and inner duct is abundant, and has very strong hydrophily, is a kind of desirable nano coating decorative material therefore.Disclosing a kind of among the CN102179184A is the preparation method of the ceramic micro filter film of separating layer with the palygorskite nano fiber, but does not add the nano-attapulgite stone coating of modifier, exists defectives such as surface property is poor, rete is easy to crack and come off inevitably.
Summary of the invention
The object of the present invention is to provide this advanced membrane material technology of ceramic membrane of expanding; Ceramic filtration membrane from multi-faceted exploitation superior performances such as perforated membrane supporter, nano coating modification, making form and occupation modes; Overcome the deficiency in the conventional art, thereby realized the object of the invention.
The technical problem that the present invention solved can adopt following technical scheme to realize:
A kind of rare earth modified attapulgite clay nano coating ceramic filter membrane; It is characterized in that, comprise ceramic supporting body, be arranged at the diffusion barrier of ceramic support surface, be arranged at the inner cavity of ceramic supporting body; Be arranged at the spout of ceramic supporting body bottom, said spout is communicated with cavity.
In one embodiment of the invention, said ceramic supporting body is circular, fan-shaped or rectangle, and the matrix face thickness is 2～6 millimeters, and cavity thickness is 2～8 millimeters, and gross thickness is 6～20 millimeters.
A kind of preparation method of rare earth modified attapulgite clay nano coating ceramic filter membrane is characterized in that it comprises the steps:
A. prepare ceramic supporting body
With the Concave-convex clay rod is major ingredient, grinds behind the interpolation rare earth oxide, adds dispersant and pore creating material again, fully stirs with water then and processes slurry, again slurry is processed ceramic idiosome, obtains ceramic supporting body to ceramic idiosome sintered heat insulating in high temperature furnace at last;
B. on ceramic supporting body, prepare diffusion barrier
With nano-attapulgite stone and oxide nano rare earth is raw material, adds dispersant, thickener and antifoaming agent then and is scattered in and processes coated film liquid in the water; The mode that again coated film liquid is lifted with dipping evenly is applied to the surface of ceramic supporting body, and after drying, drying, roasting again, cooling obtains finished product naturally.
In one embodiment of the invention, among the said step a sintered heat insulating technology for the heating rate of 1～5 ℃/min sintering and be incubated 1～5 hour in 900～1200 ℃ of scopes.
In one embodiment of the invention, the roasting technique among the said step b is roasting 1～5 hour in 650～950 ℃ temperature range.
In one embodiment of the invention, the rare earth oxide among the said step a is La
2O
3, pore creating material is polystyrene microsphere, poly (methyl methacrylate) micro-sphere or starch; The mass ratio of Concave-convex clay rod, rare earth oxide and pore creating material is 1: 0.08～0.20: 0.06～0.15.
In one embodiment of the invention, the rare earth oxide among the said step b is La
2O
3, the mass ratio of Concave-convex clay rod and rare earth oxide is 1: 0.08～0.15; The dispersant of coated film liquid is polyethylene glycol, polymethylacrylic acid or polymine; Thickener is a carboxymethyl cellulose; Methylcellulose, polyvinyl alcohol or polyethylene glycol; Antifoaming agent is a silicone defoaming agent, and wherein the mass ratio of dispersant, thickener, antifoaming agent is 1: 0.1～5: 0.1～5.
In one embodiment of the invention, the stoving process among the said step b is 70～110 ℃ of dryings 12～24 hours; Roasting technique is warming up to 550～650 ℃ of scopes and is incubated 0.5～3 hour for the speed with 0.5～5 ℃/min in high temperature furnace; Speed with 0.5～3 ℃/min is warming up to 850～950 ℃ of scopes and is incubated 1～5 hour again.
Substantive distinguishing features and obvious improvement that technical scheme of the present invention is outstanding are mainly reflected in:
(1) adopting rare earth oxide is modifier and dose; Sintering prepares that microcellular structure is good, even aperture distribution, light weight, attapulgite ceramic supporting body that intensity is high; Solved the low defective of attapulgite ceramics strength technically; When newly utilizing approach, a kind of supporter of excellent performance is provided for the ceramic filtration membrane preparation also for the attapulgite developing;
(2) adopt the natural nano attapulgite to prepare the ceramic filtration membrane separating layer, can significantly reduce the manufacturing cost of ceramic filtration membrane, La particularly mixes
2O
3Improve the coating sintering condition in the nanometer rare earth oxide powder, strengthened the density and the stability of nano coating;
(3) the present invention separates rete with nano composite material coating preparation, its rete not easy to crack with come off, the top layer nano-meter characteristic is outstanding; Have strong hydrophily and oleophobic property; Fenestra is evenly fine and close, and permeability rate is high, is difficult for being stain by oiliness and biological substance; Be more suitable for the isolated by filtration of water treatment and high protein content material, can greatly delay film and pollute;
(4) the present invention prepares the earthenware slab filter membrane with the hollow cavity structure, is to the technical expansion of the current one chip earthenware slab filter membrane that only can be applied to separate with back yard industry in the laboratory, also for ceramic membrane a kind of brand-new structural shape is provided;
(5) the novel hollow cavate earthenware slab film processed of the present invention is compared with tubular membrane or multi-channel membrane, and the loading density of film increases considerably, and the film surface clean is more prone to.Particularly this flat ceramic filtration membrane can be processed the rotary disk type membrane assembly easily; Adopt initiatively cross-flow mode rotating operation; With filtrating shearing force that relative motion produced face is formed and to wash away strongly; Realized continuous wash, very helped eliminating concentration polarization and delay film and stop up the film surface.Expection the present invention has popularizing application prospect widely in fields such as water treatment and bio-pharmaceuticals, food processing, fine chemistry industries.
Description of drawings
Below in conjunction with accompanying drawing technical scheme of the present invention is described further:
Fig. 1 is the structural representation of nano coating ceramic filtration membrane of the present invention;
Fig. 2 is the cloudy plate sketch map of nano coating ceramic filtration membrane of the present invention.
Fig. 3 is the positive plate sketch map of nano coating ceramic filtration membrane of the present invention.
Fig. 4 is the front view of nano coating ceramic filtration membrane of the present invention.
Fig. 5 is the embodiment front view of nano coating ceramic filtration membrane of the present invention.
Fig. 6 is the embodiment side view of nano coating ceramic filtration membrane of the present invention.
The specific embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect and be easy to understand and understand, below in conjunction with the specific embodiment, further set forth the present invention.
As shown in Figure 1; Rare earth modified attapulgite clay nano coating ceramic filter membrane of the present invention; Comprise ceramic supporting body 1 and the diffusion barrier 2 that is arranged at the ceramic support surface; Said ceramic supporting body set inside has cavity 3, and the bottom of ceramic supporting body is provided with spout 4, and said spout is communicated with cavity.
As shown in Figures 2 and 3, said ceramic supporting body is formed by the cloudy plate A that processes respectively and two ceramic body negative and positive of positive plate B sintering that interlocks.Its profile is 60 ° fan-shaped, and the covering of the fan radius is 35mm, matrix face thickness 3mm, cavity thickness 2mm, gross thickness 8mm.Cloudy plate A periphery is opened groove C one, and there is the semicircle column type passage D that effluents the bottom; The size of sun plate B and shape and cloudy plate A are complementary, and periphery is opened boss E one, and there is the semicircle column type passage F that effluents the bottom;
As shown in Figure 4, cloudy plate A and positive plate B accurately interlock, and form cavity 3, bottom semicircle column type effluent passage D and the tight combination of F, the spout 4 that formation communicates with cavity.
Manufacture craft of the present invention is following:
A. according to above-mentioned product requirement, the gypsum mold of cloudy plate A of processing and fabricating and positive plate B;
B. with 200 order Concave-convex clay rods, La
2O
3Powder is abrasive material in ball mill respectively, carries out the waterpower classification of sedimentation then;
C. with Concave-convex clay rod, the La of classification
2O
3Mix at 1: 0.12: 0.10 according to mass ratio with polystyrene (PS) microballoon, add composite ceramic dispersant (TH-908 type) 0.1% (solid/solid) then, in de-airing mixer, fully stir, process the mud that is suitable for injection forming with water;
D. with the ceramic mud of processing, be injected into mould, promptly get green compact after the demoulding.Adopt microwave drying technology that base substrate is carried out drying, and moisture is dropped to below 3%.With two tight fastenings of dried base substrate of yin, yang, get into the high temperature furnace sintering.The heating rate of room temperature to 500 ℃ is 1.0 ℃/min, and 500～1050 ℃ heating rate is 5.0 ℃/min, 1050 ℃ of insulations 2 hours, obtains high voidage and high-intensity attapulgite ceramic supporting body after the cooling.
E. with the nano-attapulgite stone of 30～50nm and the nanometer La of 30～50nm
2O
3Mix at 1: 0.12 according to mass ratio, join then in the aqueous solution that contains 0.3% polymine (PEI), 0.4% carboxymethyl cellulose (CMC) and 0.01% silicone defoaming agent, in ball mill, grind 20min, process the good coated film liquid of suspension;
F. adopt dip-coating method at the supporting body surface uniform coating.Keep spout to immerse coated film liquid up the ceramic supporting body of sintering preparation, at the uniform velocity mention then.After room temperature is dried, 85 ℃ of heated-air dryings 12 hours.
G. dried ceramic filtration membrane semi-finished product are put into high temperature furnace and carry out roasting, the heating rate of room temperature to 500 ℃ was 1.0 ℃/min, 500 ℃ of insulations 2.0 hours; Again with the heating rate to 900 of 2.0 ℃/min ℃, and 900 ℃ of insulations 3 hours.Naturally after the cooling, obtain the diffusion barrier of nano-modified coating, the about 20 μ m of teleblem thickness, average pore size 0.20 μ m.
Like Fig. 5 and shown in Figure 6, with the hollow cavate flat ceramic filter membrane of processing, around a rotary drum be combined into can rotating operation membrane separation plant, adopt initiatively cross-flow mode rotating operation.Membrane module forms face with filtrating shearing force that relative motion produced in rotary course and washes away strongly, can realize the continuous wash to the film surface, very helps eliminating concentration polarization and delays the film obstruction.The structure of hollow cavate also can realize backwash operation easily under necessary situation.
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; The present invention is not restricted to the described embodiments; That describes in the foregoing description and the specification just explains principle of the present invention; Under the prerequisite that does not break away from spirit and scope of the invention, the present invention also has various changes and modifications, and these variations and improvement all fall in the scope of the invention that requires protection.The present invention requires protection domain to be defined by appending claims and equivalent thereof.
Claims (8)
1. rare earth modified attapulgite clay nano coating ceramic filter membrane; It is characterized in that comprise ceramic supporting body and the diffusion barrier that is arranged at the ceramic support surface, said ceramic supporting body set inside has cavity; The bottom of ceramic supporting body is provided with spout, and said spout is communicated with cavity.
2. a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane according to claim 1; It is characterized in that said ceramic supporting body is circular, fan-shaped or rectangle, the matrix face thickness is 2～6 millimeters; Cavity thickness is 2～8 millimeters, and gross thickness is 6～20 millimeters.
3. the preparation method of a rare earth modified attapulgite clay nano coating ceramic filter membrane is characterized in that it comprises the steps:
A. prepare ceramic supporting body
With the Concave-convex clay rod is major ingredient, grinds behind the interpolation rare earth oxide, adds dispersant and pore creating material again, fully stirs with water then and processes slurry, again slurry is processed ceramic idiosome, obtains ceramic supporting body to ceramic idiosome sintered heat insulating in high temperature furnace at last;
B. on ceramic supporting body, prepare diffusion barrier
With nano-attapulgite stone and oxide nano rare earth is raw material, adds dispersant, thickener and antifoaming agent then and is scattered in and processes coated film liquid in the water; The mode that again coated film liquid is lifted with dipping evenly is applied to the surface of ceramic supporting body, and after drying, drying, roasting again, cooling obtains finished product naturally.
4. the preparation method of a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane according to claim 3; It is characterized in that sintered heat insulating technology is for the heating rate of 1～5 ℃/min sintering and be incubated 1～5 hour in 900～1200 ℃ of scopes among the said step a.
5. the preparation method of a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane according to claim 3 is characterized in that, the roasting technique among the said step b is roasting 1～5 hour in 650～950 ℃ temperature range.
6. the preparation method of a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane according to claim 3 is characterized in that, the rare earth oxide among the said step a is La
2O
3, pore creating material is polystyrene microsphere, poly (methyl methacrylate) micro-sphere or starch; The mass ratio of Concave-convex clay rod, rare earth oxide and pore creating material is 1: 0.08～0.20: 0.06～0.15.
7. the preparation method of a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane according to claim 3 is characterized in that, the rare earth oxide among the said step b is La
2O
3, the mass ratio of Concave-convex clay rod and rare earth oxide is 1: 0.08～0.15; The dispersant of coated film liquid is polyethylene glycol, polymethylacrylic acid or polymine; Thickener is a carboxymethyl cellulose; Methylcellulose, polyvinyl alcohol or polyethylene glycol; Antifoaming agent is a silicone defoaming agent, and wherein the mass ratio of dispersant, thickener, antifoaming agent is 1: 0.1～5: 0.1～5.
8. the preparation method of a kind of rare earth modified attapulgite clay nano coating ceramic filter membrane according to claim 3 is characterized in that, the stoving process among the said step b is 70～110 ℃ of dryings 12～24 hours; Roasting technique is warming up to 550～650 ℃ of scopes and is incubated 0.5～3 hour for the speed with 0.5～5 ℃/min in high temperature furnace; Speed with 0.5～3 ℃/min is warming up to 850～950 ℃ of scopes and is incubated 1～5 hour again.
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| US11040313B2 (en) | 2019-10-14 | 2021-06-22 | Huaiyin Normal University | Super-hydrophilic/underwater super-oleophobic separation membrane and preparation method thereof |
| CN111905575B (en) * | 2019-10-14 | 2022-02-11 | 淮阴师范学院 | Preparation method of oil-water separation membrane |
| CN111646775A (en) * | 2020-05-29 | 2020-09-11 | 西安工程大学 | Method for preparing sheet molecular sieve membrane support by using natural attapulgite |
| CN114146577A (en) * | 2021-12-09 | 2022-03-08 | 广西碧清源环保投资有限公司 | Ceramic filtering membrane capable of releasing negative ions and preparation method thereof |
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Application publication date: 20120801 |