CN104725071A - Preparation method of new-structure ceramic filter body for micro/nano particle filtration - Google Patents
Preparation method of new-structure ceramic filter body for micro/nano particle filtration Download PDFInfo
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- CN104725071A CN104725071A CN201510115548.5A CN201510115548A CN104725071A CN 104725071 A CN104725071 A CN 104725071A CN 201510115548 A CN201510115548 A CN 201510115548A CN 104725071 A CN104725071 A CN 104725071A
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Abstract
The invention discloses a preparation method of a new-structure ceramic filter body for micro/nano particle filtration, which comprises the following steps: 1) preparing a ceramic blank with micron-sized through pore canals; 2) carrying out rubber discharging or degreasing on the ceramic blank; and 3) calcining the honeycomb blank to obtain the ceramic filter body with micron-sized through pore canals, wherein the inner walls of the pore canals extend the crystal whisker structure. The pore wall part particles of the ceramic filter body are combined closely, the pore size is micron size, and the inner walls of the pores extend the crystal whisker. The ceramic filter body has the advantages of high temperature resistance, chemical corrosion resistance and the like, is suitable for filtering and purifying multiple fluids, including gases, liquids and the like, and is especially suitable for filtering and purifying micro/nano particles in the fluids. The preparation method has the advantages of simple technique and low facility request.
Description
Technical field
The present invention relates to field of material technology, particularly, relate to one and have the preparation method of the ceramic filtering body of " micron order clear opening, duct inner wall extend whisker " structure.
Background technology
Ceramic honey comb has parallel through pore texture, have that osmotic pressure is high, geometric jacquard patterning unit surface is large, diffusion length is short, be conducive to counting of particle and discharge with gas and to reduce advantages such as filtering volume, have a wide range of applications in the purifying treatment etc. of the filtration, purification of industrial gaseous waste, motor-vehicle tail-gas and other life waste gas, the heat exchange of metallurgical industry and the filtration of molten metal, the toxic gas of mining industry and liquid.Along with going from bad to worse of environment, the filtration for micro-nano particle thing in various fluid is had higher requirement to filtering bodies with purification.
Mostly current ceramic honey comb product is to be prepared from by extrusion moulding, namely the first size according to required honeycomb hole and shape (trilateral, rhombus, rectangle, hexagon etc.) prepare mould, then prepare the ceramic honey comb of duct arrangement high-sequential by the extrusion of ceramic size.Due to the restriction by mould size, the up-to-date ceramic honey comb product of Corning company of the U.S. can prepare 1200 through holes at most on the cross section of 1 square inch, be the limit that current known the method can prepare ceramic honey comb aperture, be still difficult to meet the filtration to micro-nano particle thing and enrichment.
On the other hand, namely the aperture of enable further reduction ceramic honey comb is reduced to micron dimension, its aperture reduce the increase suddenly that gas will be caused by resistance, thus reduce its working efficiency.That is, single honeycomb structure is relied on to be difficult to the small-bore required by the filtration of solution subparticle and to keep air-flow this contradiction unimpeded simultaneously.
Ceramic whisker because of crystalline structure more complete, subsurface defect is few, and its strength and modulus, all close to ideal crystal, is mainly used to activeness and quietness metal, pottery and macromolecular material.Modal whisker has Si
3n
4, SiC, Al
2o
3deng.In the preparation research of whisker, investigator is had to propose to utilize hole growth in situ whisker, as patent CN102251284A (a kind of method preparing beta-alumina whisker), and document (Ji Xiaoli, Xu Fei, power is national, Wan Weiwei, On In-situ Synthesis of Mullite Whisker strengthens foam silicon carbide ceramics, Chinese powder technology, 2011,17 (3): 33-36) and document (Lv Chenjing, Tian Xiushu, Han Yufang, fabricated in situ contains Al
2o
3whisker Al
2o
3the research of/Ti-Al matrix material mechanism), former concerns is in the preparation of whisker, and rear both pay close attention to the reinforced effects of whisker to matrix or foam base plate.Porous body prepared by above document and the hole in parts are closed pore, are difficult to use in filtration.
Patent of the present invention proposes a kind of new texture of clear opening inner wall extend whisker, not only overcomes legacy cellular pottery working efficiency to the dependence of aperture and unit surface hole count, and effectively increases the filtration of pottery to fine particle, ensure the unimpeded of fluid simultaneously.
Summary of the invention
The invention provides the preparation method of new structure ceramic filtering bodies of a kind of micron order duct, duct inner wall extend whisker, comprise the following steps.
1) preparation has the ceramic body also drying of the straight through hole of micron order.
2) organic eliminating is carried out to dried base substrate.
3) burning ceramics base substrate, obtain micron order aperture, body portion particle combines closely, hole inner wall extend has the new structure ceramic filtering bodies of whisker.
Wherein, the ceramic raw material in step 1) can be Al
2o
3, Si
3n
4, SiC, and with other powders as Si powder, carbon dust etc. can obtain Si for raw material by reaction sintering
3n
4or the powder raw material of SiC.Corresponding sintering agent, dispersion agent is added according to different raw materials; Corresponding shaping medium is added according to different forming methods.
Wherein, the ceramic body in step 1) with micron order clear opening adopts ionic gel or freeze-drying preparation.Ionic gel technology is as document (Rosemarie Dittrich, Gerhard Tomandl, Martina Mangler, Preparation of Al2O3, TiO2, and Hydroxyapatite Ceramics with Pores Similar to a Honeycomb Structure) (Dittrich R, Tomandl G, Scaffolds for Hard Tissue Engineering by Ionotropic Gelation of Alginate-Influence of Selected Preparation Parameters) (Ahmed A. Eljaouhari, et al., New Anisotropic Ceramic Membranes from Chemically Fixed Dissipative Structures) (Long Menglong, Ma Ning, Yang Jinlong, the preparation of aperture controlled micron order aluminum oxide clear opening pottery) described in, freeze-drying is as document (Li J, Zuo KH, Zhang FQ, et al., The controllable Microstructure of Porous Al2O3 Ceramics Prepared via a Novel Freeze Casting Route) (Araki K, Halloran JW, Porous Ceramic Bodies with Interconnected Pore Channels by a Novel Freeze Casting Technique) (Li Lijuan, Dong Yinsheng, Lin Pinghua, storage is grown into forest, Sheng Xiaobo, Guo Chao, orienting stephanoporate pottery is prepared in directional freeze and lyophilize) described in.The aperture of the honeycomb body obtained after drying is at 10 μm-200 μm, and hole depth is at 10mm-200mm.
Ceramic material powder involved in the present invention, sintering agent powder and the additive such as dispersion agent, shaping medium are common commercial powder, its purity is commercial level, but further according to adjusting the requirement of product purity, also can adopt the grade reagents such as analytical pure.
The powder granularity of raw alumina powder involved in the present invention, sintering agent powder and dispersion agent, shaping medium etc. is more little is more conducive to shaping and sintering, preferably less than 2.0 μm powders, but is not limited thereto scope.
In the inventive method, step 2) in the drying of honeycomb body be lyophilize, keep the parallel construction in honeycomb duct in base substrate.
Step 2) in organism eliminating is carried out to dried base substrate, temperature is at 500 DEG C ~ 800 DEG C, and the time is 0.5 ~ 3 h.
In the inventive method, calcined by honeycomb body in step 3), calcining temperature is 1200 DEG C ~ 1600 DEG C, insulation 1h ~ 3h.Different calcining temperatures and time is selected according to different ceramic raw materials.
The present invention proposes on the framework of ceramic honey comb base substrate, utilizes hole to grow the principle of whisker, prepares the ceramic honey comb that hole wall is " whisker intert parallel channels " novel texture of whisker.The whisker stretched in this novel texture cellular alumina ceramic channel walls effectively can carry out the filtration of fine particle, and its original basic honeycomb parallel via holes structure in turn ensure that the smoothness of fluid.
The present invention is based on hole provides space can the principle of growth in situ whisker, by controlling the sintering condition of ceramic body or adding catalyzer, prepares the new texture ceramic honey comb of " duct inner wall extend whisker ".The present invention, according to the pattern feature of whisker, utilizes the whisker of duct inner wall extend to increase filtration to fine particle, utilizes parallel channels to ensure the unimpeded of fluid simultaneously, overcomes the dependence of legacy cellular pottery working efficiency to aperture and unit surface hole count.The present invention first at honeycomb structure situ synthesizing whisker, and develops whisker and is filtering and the new opplication of field of purification in conjunction with honeycomb structure.
By the ceramic honey comb that method of the present invention is prepared, there is the premium propertiess such as high temperature resistant, resistance to chemical attack, be applicable to filtration and the purification of multiple fluid, as the filtration, purification of fine particle in air, waste gas that various commercial run produces, its other life waste gas of motor-vehicle tail-gas, also can be used for the tabular adsorbent of analysis chromatographic column, to the filtration of the heat exchange of metallurgical industry and molten metal, to the toxic gas of mining industry and the purifying treatment etc. of liquid.Scanning electron microscope (SEM) shows ceramic honey comb body portion particle of the present invention and combines closely, and honeycomb hole inwall grows into whisker, forms parallel channels.This structure makes ceramic honey comb of the present invention can be kept the smoothness of fluid in use by straight channels, and the whisker of passing hole channel inner wall extend filters further, cleansing fluid.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.Without departing from the spirit and substance of the case in the present invention, the amendment do the inventive method, step or condition or replacement, all belong to scope of the present invention.
If do not specialize, chemical feedstocks used in embodiment is conventional commercial raw material, the conventional means that technique means used in embodiment is well known to those skilled in the art.
the preparation of embodiment 1 new texture silicon nitride ceramics filtering bodies.
1g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 1%.In sodium alginate soln, add 15g beta-silicon nitride powder, add Y
2o
30.75g and Y
2o
30.3g is as sintering agent, and the 1wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, and vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, the base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, and after dry, sample is placed in draft glue discharging furnace, 650 DEG C of insulation 2h organics removal.Base substrate after binder removal is put into sintering oven, is warming up to 1750 DEG C with speed 10 DEG C/min, under the nitrogen pressure of 0.5MPa, sinters 2.5h, be there is the silicon nitride honeycomb pottery of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon nitride honeycomb pottery is 69%, aperture is that about 120 μm and whisker length are scope 5 μm ~ 80 μm.
the preparation of embodiment 2 new texture silicon nitride ceramics filtering bodies.
1.5g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 1.5%.In sodium alginate soln, add 15g beta-silicon nitride powder, add Y
2o
30.75g and Y
2o
30.3g is as sintering agent, and the 1wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, and vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, the base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, and after dry, sample is placed in draft glue discharging furnace, 650 DEG C of insulation 2h organics removal.Base substrate after binder removal is put into sintering oven, is warming up to 1850 DEG C with speed 10 DEG C/min, under the nitrogen pressure of 0.5MPa, sinters 2.5h, be there is the silicon nitride honeycomb pottery of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon nitride honeycomb pottery is 65%, aperture is that about 50 μm and whisker length are scope 5 μm ~ 30 μm.
the preparation of embodiment 3 new texture silicon nitride ceramics filtering bodies.
1g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 1%.In sodium alginate soln, add 5g silicon powder, and the 1wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, after dry, sample is placed in tube furnace, sinter 2.5h with 10 DEG C/min ramp to 1350 DEG C under nitrogen atmosphere, be there is the silicon nitride honeycomb pottery of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon nitride honeycomb pottery is 78%, aperture is that about 500 μm and whisker length are scope 100 μm ~ 400 μm.
the preparation of embodiment 4 new texture silicon nitride ceramics filtering bodies.
0.5g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 0.5%.In sodium alginate soln, add 20g silicon powder, and the 1wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, after dry, sample is placed in tube furnace, sinter 2.5h with 10 DEG C/min ramp to 1400 DEG C under nitrogen atmosphere, be there is the silicon nitride honeycomb pottery of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon nitride honeycomb pottery is 78%, aperture is that about 550 μm and whisker length are scope 300 μm ~ 400 μm.
the preparation of embodiment 5 new texture silicon carbide ceramics filtering bodies.
0.5g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 0.5%.In sodium alginate soln, add 15g silicon carbide powder, add Y
2o
30.15g and Y
2o
30.3g is as sintering agent, and the 0.8wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, and vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1.5M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, the base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, and after dry, sample is placed in draft glue discharging furnace, 650 DEG C of insulation 2h organics removal.Base substrate after binder removal is put into sintering oven, is warming up to 1650 DEG C of sintering 2.5h with speed 10 DEG C/min under nitrogen atmosphere, be there is the silicon carbide honeycomb ceramics of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon carbide honeycomb ceramics is 70%, aperture is that about 350 μm and whisker length are scope 50 μm ~ 200 μm.
the preparation of embodiment 6 new texture silicon carbide ceramics filtering bodies.
1g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 1%.In sodium alginate soln, add 10g silicon carbide powder, add Y
2o
30.1g and Y
2o
30.2g is as sintering agent, and the 0.8wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, and vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1.5M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, the base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, and after dry, sample is placed in draft glue discharging furnace, 650 DEG C of insulation 2h organics removal.Base substrate after binder removal is put into sintering oven, is warming up to 1650 DEG C of sintering 2.5h with speed 10 DEG C/min under nitrogen atmosphere, be there is the silicon carbide honeycomb ceramics of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon carbide honeycomb ceramics is 73%, aperture is that about 280 μm and whisker length are scope 50 μm ~ 200 μm.
the preparation of embodiment 7 new texture alumina-ceramic filtering bodies.
2g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 2%.In sodium alginate soln, add 15g alumina powder jointed, add CaF
20.47g and kaolin 0.17g is as sintering agent, and the 0.3wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, and vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1.5M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, the base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, and after dry, sample is placed in draft glue discharging furnace, 650 DEG C of insulation 2h organics removal.Base substrate after binder removal is put into sintering oven, is being warming up to 1580 DEG C of sintering 2.5h with speed 10 DEG C/min, be there is the cellular alumina pottery of " duct inner wall extend whisker " structure.In this embodiment, the void content of cellular alumina pottery is 68%, aperture is that about 20 μm and whisker length are scope 0.5 μm ~ 10 μm.
the preparation of embodiment 8 new texture alumina-ceramic filtering bodies.
1.5g sodium alginate is added in 100mL distilled water, fully stir the homogeneous solution being mixed with 2%.In sodium alginate soln, add 20g alumina powder jointed, add CaF
20.62g and kaolin 0.21g is as sintering agent, and the 0.3wt% Triammonium citrate adding powder quality is as dispersion agent, fully stirs, after ceramic size being placed in ball grinder ball milling 5h, and vacuum stripping 30min in vacuum rotary evaporator.Slurry is injected the glass culture dish scribbling 4% sodium alginate soln in advance, spray the calcium chloride solution 3ml of concentration 1.5M to pulp surface, leave standstill 3 days.Afterwards, the demoulding also excises the film of billet surface, soaks 1 day, take out and also clean with distilled water in the Gluconolactone solution of 1M.Wet base is placed in refrigerator and cooled and freezes 24h, the base substrate after freezing is placed in freeze drier lyophilize 24h under-50 DEG C of conditions with 20Pa, and after dry, sample is placed in draft glue discharging furnace, 650 DEG C of insulation 2h organics removal.Base substrate after binder removal is put into sintering oven, is being warming up to 1600 DEG C of sintering 2.5h with speed 10 DEG C/min, be there is the cellular alumina pottery of " duct inner wall extend whisker " structure.In this embodiment, the void content of silicon carbide honeycomb ceramics is 65%, aperture is that about 50 μm and whisker length are scope 0.5 μm ~ 20 μm.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1., for a preparation method for the new structure ceramic filtering bodies of micro-nano particle thing filtration, it is characterized in that, described method comprises the following steps:
1) preparation has the ceramic body also drying of the micron order level clear opening of 15 μm of-600 μm of scopes;
2) organic eliminating is carried out to dried base substrate;
3) burning ceramics base substrate, obtain wall portion particle and combine closely, pore diameter range is at 15 μm-600 μm and hole inner wall extend has length in the new structure ceramic filtering bodies of the whisker of 0.5 μm of-300 μm of scope.
2. preparation method as claimed in claim 1, is characterized in that, the ceramic body in step 1) with the micron order clear opening of 15 μm of-600 μm of scopes adopts Ionic gelation method preparation.
3. preparation method as claimed in claim 1, is characterized in that, the ceramic body in step 1) with the micron order clear opening of 15 μm of-600 μm of scopes adopts freeze-drying preparation.
4. the method for claim 1, is characterized in that, step 2) in organism eliminating is carried out to dried base substrate, temperature is at 500 DEG C ~ 800 DEG C, and the time is 0.5 ~ 3 h.
5. the method for claim 1, is characterized in that, in step 3), calcining temperature is 1200 DEG C ~ 1600 DEG C, insulation 1 ~ 3 h.
6. the preparation-obtained new structure ceramic filtering bodies with the micron order clear opening of 15 μm of-600 μm of scopes, the whisker of duct inner wall extend length 0.5 μm of-300 μm of scope of the preparation method according to the arbitrary claim of claim 1-5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111099919A (en) * | 2020-01-14 | 2020-05-05 | 中国人民解放军国防科技大学 | Silicon nitride ceramic with hierarchical pore structure and preparation method thereof |
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| CN104072141A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Preparation method of silicon carbide honeycomb ceramics |
| CN104072148A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Low-cost preparation method of silicon nitride honeycomb ceramics |
| CN104072111A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Preparation method of aluminium oxide honeycomb ceramics |
| CN104072147A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Preparation method of silicon nitride honeycomb ceramics |
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| CN104072141A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Preparation method of silicon carbide honeycomb ceramics |
| CN104072148A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Low-cost preparation method of silicon nitride honeycomb ceramics |
| CN104072111A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Preparation method of aluminium oxide honeycomb ceramics |
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| CN111099919A (en) * | 2020-01-14 | 2020-05-05 | 中国人民解放军国防科技大学 | Silicon nitride ceramic with hierarchical pore structure and preparation method thereof |
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Application publication date: 20150624 |