CN100439293C - Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method - Google Patents
Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method Download PDFInfo
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- CN100439293C CN100439293C CNB2007100217117A CN200710021711A CN100439293C CN 100439293 C CN100439293 C CN 100439293C CN B2007100217117 A CNB2007100217117 A CN B2007100217117A CN 200710021711 A CN200710021711 A CN 200710021711A CN 100439293 C CN100439293 C CN 100439293C
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Abstract
This invention discloses a porous ceramic filtration plate coated with nanoscale ceramic filtration film for liquid-solid separation. The nanoscale ceramic filtration film is prepared by: hydrolyzing aluminum isopropoxide, preparing a sol with HNO3, refluxing, aging to form aluminum sol, adding Al2O3 nanopowder, mixing, dispersing to form uniform nanoscale film gel, uniformly coating onto the surface of a substrate by Czochralski method, drying and sintering. The obtained porous ceramic filtration plate can effectively block the majority of fine particles in ore slurry, and has such advantages as no blockage, long service life and wide applications.
Description
Technical field
The invention belongs to the solid-liquid separation field, relate to filter plate of porous ceramic, refer in particular to the filter plate of porous ceramic that a kind of surface-coated has Nano ceramic membrane filter, be specially adapted to pulp dewatering and filter, provide the manufacture method of this filter plate of porous ceramic simultaneously.
Background technology
As filtration medium, the ceramic filter plate of ceramic filter in use micropore can be blocked, the factor that causes the ceramic filter plate obstruction is a lot, wherein one of topmost factor is the subparticle that contains in the ore pulp, can enter in the filtration duct of ceramic membrane along with filtering process, thereby cause that the ceramic filter plate filtration capacity declines to a great extent.
For preventing that the ceramic filter plate filtration capacity from weakening, the ceramic filter chance is carried out periodically matting and ultrasonic cleaning to it, make it return to higher filtration vessel levels, but, this cleaning is not completely, the material that still has small part is residual, so along with the accumulation of tamper, ceramic plate thoroughly can be blocked and scrap.
Existing ceramic filter plate all uses the micron order ceramic filter membrane, subparticle in the ore pulp very easily enters in the duct of ceramic membrane, thereby cause above-mentioned obstruction process, can have a strong impact on the one hand the work-ing life of ceramic filter plate, existing ceramic plate average work-ing life is about 1 year.Limited the use field of ceramic plate on the other hand, the ore pulp thinner to some granularities, micron-sized ceramic membrane just can't be suitable for.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, provide a kind of surface-coated that the filter plate of porous ceramic of Nano ceramic membrane filter is arranged, can effectively stop exhausted most fine particle in the ore pulp, thereby it is blocked that ceramic plate is difficult for, and can prolong the work-ing life of ceramic plate well.On the other hand, the ore pulp thinner to some granularities, this filter plate of porous ceramic still can well be suitable for, and has widened the field that ceramic filter uses effectively.Specifically implement like this: a kind of filter plate of porous ceramic that is covered with Nano ceramic membrane filter, comprise ceramic substrate and surperficial overlay film thereof, it is characterized in that overlay film is a Nano ceramic membrane filter, the raw material each component weight proportion of Nano ceramic membrane filter is:
100 parts of deionized waters
Aluminum isopropylate analytical pure 1-3 part
Nano alumina powder 2-4 part
The pure 0.1-0.5 part of 10%HNO3 solution chemistry.
The Nano ceramic membrane filter of filter plate of porous ceramic surface-coated of the present invention adopts the ultimate principle of sol-gel method, promptly uses aluminum isopropylate as presoma, with the water reaction, generates γ-AlOOH precipitation, forms aluminium colloidal sol through the peptizing agent peptization.
With aluminum isopropylate is that the hydrolysis reaction that presoma prepares boehmite sol is:
Al(C
3H
7O)
3+H
2O→Al(C
3H
7O)
2(OH)+C
3H
7OH
Al(C
3H
7O)
2(OH)+H
2O→Al(C
3H
7O)(OH)
2+C
3H
7OH
Along with the generation of hydroxyl, aggregation further takes place, aggregation has dehydration polyreaction and dealcoholysis polyreaction, is respectively,
Dehydration polymerization: Al (C
3H
7O)
2(OH)+Al (C
3H
7O)
2(OH) → (C
3H
7O)
2-Al-O-Al-(C
3H
7O)
2+ H
2O
Dealcoholysis polymerization: Al (C
3H
7O)
3+ Al (C
3H
7O)
2(OH) → (C
3H
7O)
2-Al-O-Al-(C
3H
7O)
2+ C
3H
7OH
The result of these reactions has formed " Al-O-Al " key bridge, has constituted Al
2O
3The skeleton of pottery, agglomeration process is proceeded, and the cross-linking density of Al-O-Al is increased, up to producing gel or γ-AlOOH precipitation.Under the effect of peptizing agent, make precipitation or gel disperse to form aluminium colloidal sol again, hydrolysis and cohesion are tended towards stability, form metastable colloidal sol by reflux digestion.
Then colloidal sol is coated in the supporting body surface of making in advance, the particle generation crosslinked action in the colloidal sol forms gel, stays a large amount of small pores by drying in gel-film, forms porous ceramics coating base substrate, makes gel-film finally form Al through burning till
2O
3Ultra-filtration membrane.
Adopt the inorganic ceramic film of sol-gel method preparation; in dry and sintering process, usually can produce some tiny cracks and pin hole; in order to reduce or avoid the generation of tiny crack effectively; add organic binder bond polyvinyl alcohol (PVA) in the material component of ceramic membrane; effect is more satisfactory; with 100 parts of deionized waters is benchmark, and the add-on of polyvinyl alcohol (PVA) is 0.05-0.15 part.
Making this method that is covered with the filter plate of porous ceramic of Nano ceramic membrane filter is: carry out peptization with 10%HNO3 solution by proportioning after with the aluminum isopropylate hydrolysis, reflux digestion forms aluminium colloidal sol then, adding nano alumina powder in aluminium colloidal sol mixes, disperses, form the nanometer film gel of uniformity, adopt dip-coating method that the nanometer film gel evenly is coated on substrate surface, drying, burn till and form.
Wherein the preparation of aluminium colloidal sol is:
A. the hydrolysis of aluminium salt: deionized water is heated to 80-90 ℃, and constant temperature adds aluminum isopropylate, and the above back of magnetic agitation 1.5h is static, slowly forms precipitation;
B. peptization: be warming up to 85-95 ℃, behind the volatilization Virahol, constant temperature adds 10%HNO
3Solution disperses precipitation as peptizing agent again;
C. reflux digestion: solution is poured into reflux, greater than 24h, store for future use at 85～95 ℃ of following reflux digestions.The preparation of nanometer film gel is:
By evaporation or add water and change the aluminium collosol concentration, promptly regulate feed liquid be solid content be 4～5% can homodisperse system, in aluminium colloidal sol, add nano alumina powder and mix, disperse, the nanometer film gel of formation uniformity.
In order to prevent that Nano ceramic membrane filter from producing tiny crack and pin hole in dry and sintering process, the present invention adds PVA solution in the slurry of making, more than the ultrasonic dispersing 2h, use more than the magnetic stirrer 2h again, and then enter filming process.
The dip-coating method plated film is conventional operation method with plastic film, and operation is:
A. remove the substrate surface pollutent, keep the smooth smooth and clean of dipping face;
B. add small amount of ethanol and remove bubble in the slurry;
C. again supporter (substrate) is immersed in the slurry, slowly take out behind the dipping certain hour.
The drying of goods behind the plated film:
Goods more than 40 ℃ of dry 6h of constant temperature, are warming up to more than 100 ℃ of dry 2h again.
Dry article is burnt till: goods are placed kiln, be warming up to 450 ℃ in 5-8 hour, be warming up to 1200-1400 ℃ at 8-11 hour then, insulation 2 naturally cools to room temperature to 3h.
The present invention has effectively stopped exhausted most fine particle in the ore pulp by at filter plate of porous ceramic surface-coated Nano ceramic membrane filter, and ceramic plate is difficult for blocked, has prolonged the work-ing life of ceramic plate, has widened the field that ceramic filter uses.
Embodiment
Embodiment 1, a kind of filter plate of porous ceramic that is covered with Nano ceramic membrane filter, the surface-coated of ceramic substrate has Nano ceramic membrane filter, this Nano ceramic membrane filter is by 100 parts of deionized waters, 1 part of analytical pure aluminum isopropylate, 4 parts of nano alumina powders, 0.3 part of chemical pure 10%HNO3 solution composition, and concrete manufacture method is:
1. the preparation of Nano ceramic membrane filter:
(1) preparation of aluminium colloidal sol:
A. the hydrolysis of aluminium salt: deionized water is heated to 80-90 ℃, and constant temperature adds aluminum isopropylate, and the above back of magnetic agitation 1.5h is static, slowly forms precipitation;
B. peptization: be warming up to 85-95 ℃, behind the volatilization Virahol, constant temperature adds 10%HNO
3Solution disperses precipitation as peptizing agent again;
C. reflux digestion: solution is poured into reflux, greater than 24h, store for future use at 85～95 ℃ of following reflux digestions;
(2) preparation of nanometer film gel:
By evaporation or add water and change the aluminium collosol concentration, promptly regulate feed liquid be solid content be 4～5% can homodisperse system, in aluminium colloidal sol, add nano alumina powder and mix, disperse, the nanometer film gel of formation uniformity.
2. dip-coating method plated film:
A. remove the ceramic base plate surface pollutent, keep the smooth smooth and clean of dipping face;
B. add small amount of ethanol and remove bubble in the slurry;
C. again supporter (substrate) is immersed in the slurry, slowly take out behind the dipping certain hour.
3. product dried behind the plated film:
Goods more than 40 ℃ of dry 6h of constant temperature, are warming up to more than 100 ℃ of dry 2h again.
4. dry back goods burn till: goods are placed kiln, be warming up to 450 ℃ in 5-8 hour, be warming up to 1200-1400 ℃ at 8-11 hour then, insulation 2 naturally cools to room temperature to 3h.
Embodiment 2, a kind of filter plate of porous ceramic that is covered with Nano ceramic membrane filter, the surface-coated of ceramic substrate has Nano ceramic membrane filter, this Nano ceramic membrane filter by 100 parts of deionized waters, 2 parts of analytical pure aluminum isopropylates, 2 parts of nano alumina powders, 0.5 part of chemical pure 10%HNO3 solution, 0.1 part
PVAForm, concrete manufacture method wherein after the nanometer film preparing gel is good, adds PVA solution with embodiment 1, more than the ultrasonic dispersing 2h, uses more than the magnetic stirrer 2h again, and then enters filming process.
Embodiment 3, a kind of filter plate of porous ceramic that is covered with Nano ceramic membrane filter, the surface-coated of ceramic substrate has Nano ceramic membrane filter, this Nano ceramic membrane filter by 100 parts of deionized waters, 3 parts of analytical pure aluminum isopropylates, 3 parts of nano alumina powders, 0.1 part of chemical pure 10%HNO3 solution, 0.15 part
PVAForm, concrete manufacture method is with embodiment 2.
Embodiment 4, a kind of filter plate of porous ceramic that is covered with Nano ceramic membrane filter, the surface-coated of ceramic substrate has Nano ceramic membrane filter, this Nano ceramic membrane filter by 100 parts of deionized waters, 2 parts of analytical pure aluminum isopropylates, 3 parts of nano alumina powders, 0.4 part of chemical pure 10%HNO3 solution, 0.05 part
PVAForm, concrete manufacture method is with embodiment 2.
Claims (9)
1. a filter plate of porous ceramic that is covered with Nano ceramic membrane filter comprises ceramic substrate and surperficial overlay film thereof, it is characterized in that overlay film is a Nano ceramic membrane filter, and the raw material each component weight proportion of Nano ceramic membrane filter is:
100 parts of deionized waters
Aluminum isopropylate analytical pure 1-3 part
Nano alumina powder 2-4 part
The pure 0.1-0.5 part of 10%HNO3 solution chemistry.
2. filter plate of porous ceramic according to claim 1 is characterized in that adding the organic binder bond polyvinyl alcohol in the material component of nano ceramics film, is benchmark with 100 parts of deionized waters, and the add-on of polyvinyl alcohol is 0.05-0.15 part.
3. manufacture method that is covered with the filter plate of porous ceramic of Nano ceramic membrane filter, it is characterized in that carrying out peptization with 10%HNO3 solution after with the aluminum isopropylate hydrolysis by claim 1 or 2 described proportionings, reflux digestion forms aluminium colloidal sol then, adding nano alumina powder in aluminium colloidal sol mixes, disperses, form the nanometer film gel of uniformity, adopt dip-coating method that the nanometer film gel evenly is coated on substrate surface, drying, burn till and form.
4. manufacture method according to claim 3 is characterized in that the preparation of aluminium colloidal sol is:
A. the hydrolysis of aluminium salt: deionized water is heated to 80-90 ℃, and constant temperature adds aluminum isopropylate, and the above back of magnetic agitation 1.5h is static, slowly forms precipitation;
B. peptization: be warming up to 85-95 ℃, behind the volatilization Virahol, constant temperature adds 10%HNO
3Solution disperses precipitation as peptizing agent again;
C. reflux digestion: solution is poured into reflux, greater than 24h, store for future use at 85～95 ℃ of following reflux digestions.
5. manufacture method according to claim 3 is characterized in that the preparation of nanometer film gel comprises:
By evaporation or add water and change the aluminium collosol concentration, promptly regulate feed liquid be solid content be 4～5% can homodisperse system.
6. manufacture method according to claim 5 is characterized in that adding PVA solution in the nanometer film gel, more than the ultrasonic dispersing 2h, uses more than the magnetic stirrer 2h again.
7. manufacture method according to claim 3 is characterized in that the dip-coating method plated film is:
A. remove the substrate surface pollutent, keep the smooth smooth and clean of dipping face;
B. add small amount of ethanol and remove bubble in the slurry;
C. again substrate is immersed in the slurry, slowly take out behind the dipping certain hour.
8. manufacture method according to claim 3, it is characterized in that behind the plated film drying of goods be with goods more than 40 ℃ of dry 6h of constant temperature, be warming up to again more than 100 ℃ of dry 2h.
9. manufacture method according to claim 3 is characterized in that dry article burns till to goods are placed kiln, is warming up to 450 ℃ in 5-8 hour, is warming up to 1200-1400 ℃ at 8-11 hour then, and insulation 2 naturally cools to room temperature to 3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100217117A CN100439293C (en) | 2007-04-20 | 2007-04-20 | Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method |
Applications Claiming Priority (1)
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|---|---|---|---|
| CNB2007100217117A CN100439293C (en) | 2007-04-20 | 2007-04-20 | Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101092307A CN101092307A (en) | 2007-12-26 |
| CN100439293C true CN100439293C (en) | 2008-12-03 |
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| CNB2007100217117A Expired - Fee Related CN100439293C (en) | 2007-04-20 | 2007-04-20 | Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method |
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| CN102746022B (en) * | 2011-12-29 | 2013-12-04 | 西安建筑科技大学 | Preparation method for Al2O3 ceramic material having controllable bimodal porous structure |
| CN103482998B (en) * | 2012-06-15 | 2015-05-13 | 南京理工大学 | Preparation method of tubular tin dioxide ceramic membrane |
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| CN104774024B (en) * | 2015-04-16 | 2017-05-24 | 柳州豪祥特科技有限公司 | Preparation process of tubular water treatment membranes |
| CN105957999B (en) * | 2016-07-05 | 2019-09-13 | 东莞市卓高电子科技有限公司 | A kind of PE diaphragm of dopen Nano ceramic particle and preparation method thereof |
| CN107973615B (en) * | 2016-10-24 | 2020-12-18 | 天津工业大学 | Mesoporous gamma-Al2O3Ceramic membrane and preparation method thereof |
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| CN111517766A (en) * | 2020-05-11 | 2020-08-11 | 镇江华鑫磨具有限公司 | Method for manufacturing porous ceramic filter plate |
| CN113772704A (en) * | 2021-09-13 | 2021-12-10 | 中山大学 | Preparation method of two-dimensional alumina powder |
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| Publication number | Publication date |
|---|---|
| CN101092307A (en) | 2007-12-26 |
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Application publication date: 20071226 Assignee: Jiangsu Philip Environmental Protection Engineering Co., Ltd. Assignor: Jiangsu Prov. Ceramic Research Inst. Co., Ltd. Contract record no.: 2010320000316 Denomination of invention: Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method Granted publication date: 20081203 License type: Exclusive License Record date: 20100329 |
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