CN1807355A - Porous ceramics preparation method - Google Patents
Porous ceramics preparation method Download PDFInfo
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- CN1807355A CN1807355A CN 200510027087 CN200510027087A CN1807355A CN 1807355 A CN1807355 A CN 1807355A CN 200510027087 CN200510027087 CN 200510027087 CN 200510027087 A CN200510027087 A CN 200510027087A CN 1807355 A CN1807355 A CN 1807355A
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Abstract
The invention relates to a preparation method for porous ceramic with flocculant. Wherein, stirring to aggregate the distributed ceramic powder in water phase and form the porous structure by equal depositing and stacking. The product has porosity can come up to more than 50% and unit weight about 1g/cm3 used for filter and carrier. This invention is simple and low cost.
Description
Technical field
The present invention relates to the preparation method of pottery, relate in particular to a kind of method that flocculation agent prepares porous ceramics of introducing.
Background technology
At present, the technology of existing preparation porous ceramics is many, and technology generally has the organic foam precursor process, adds pore-forming material method, foaming, particle packing method etc.The organic foam precursor process can not reach the porous ceramics of making micrometer grade hole; The void ratio that adds the prepared porous ceramics of pore-forming material method and foaming is more inhomogeneous, can not connect continuously between the Kong Yukong of the porous ceramics of making aspect some, and foaming mostly is the hole of holding one's breath; Use the porous ceramics of particle packing method preparation, void distribution is more even, can form the hole of multiple pore size and connection, but owing to relating to molding particles and adding technological process such as binding agent compression moulding, whole technological process more complicated.
Summary of the invention
At the shortcoming of prior art, the invention provides a kind of novel method for preparing porous ceramics, higher to make voidage, porous nickel has better pore connectivity, and intensity is good, and strainability is stable, porous ceramics with low cost.
The technical solution adopted in the present invention comprises the steps:
1, a gets powder: aluminum oxide 20～23 grams, kaolin 8～9 grams, Feldspar Powder 20～22 grams; Add 5～8 gram ethanolic solns and make defoamer; Powder is preferably 100～300 orders.
B adds suitable quantity of water earlier and stirs, and adding the mass ratio that is no less than 50g while stirring then is the polyacrylamide solution of 0.1%～1% (being preferably 0.3%), makes it flocculation sediment;
C continues to stir 5～6 minutes, and the speed of stirring is 200～600 commentaries on classics/min.
By regulating the porous ceramics that different rotating speeds can prepare different porosities, strengthen rotating speed and help producing the porous ceramics that porous nickel distributes more.
2, moulding: on beaker, add a slice wire netting, mould is placed on the wire netting, with slip casting method slurry is injected mould then, need not pressurize, leave standstill, can flow away between wire netting at the inner unnecessary polyacrylamide solution of base substrate.
3, drying: it is slowly dry to be placed on shady and cool place, and unsuitable drying is too fast, and stronger ventilation condition had better not be arranged, and allows the base substrate seasoning, prevents because strong capillary action is shunk base substrate, to keep inner space.
4, sintering: sintering temperature and time are as follows:
80～500℃ 105min
500 ℃ of insulation 30min
500～950℃ 45min
950 ℃ of insulation 60min
950～1200℃ 25min
1200 ℃ of insulation 120min
Further improved technical scheme of the present invention is:
In the powder of step 1, increase a small amount of calcium carbonate powders; And behind flocculation sediment, stir certain hour, adding an amount of mass ratio rapidly then is the Al (H of 5%～35% (being preferably 30%)
2PO
4)
3The aqueous solution 5～10g continues to stir again, and churning time was no more than for 20 seconds.
In ceramic powder, add a spot of calcium carbonate superfine powder powder, in the process of flocculation, add an amount of aluminium dihydrogen phosphate, the bubble that makes its generation is unlikely to because secular stirring and fragmentation, the voidage height of the porous ceramics that the hole of the porous ceramics of making can prepare than flocculence only.
Beneficial effect
1, the present invention creatively introduces the use flocculation agent, by stirring, aqueous phase dispersive ceramic powder is reunited, pile up by uniform settling in liquid phase, thus the vesicular structure of formation high porosity;
2, the big I of agglomerating particles is by regulating the speed that stirs, and different churning time can form different particles dispersed effects;
3, moulding process is simple, only need get final product by injection forming in mould, and have the advantage of particle packing method, but save the mechanical-moulded process of particulate, and is with low cost;
4, void distribution is more even, and the porosity of the porous ceramic film material of making can reach more than 50%, and unit weight is at 1g/cm
3About.
5, owing to have a high porosity, percentage of open area preferably, the porous ceramics of this method preparation can be used for filtering.Confirm that by experiment the precipitation of calcium carbonate that generates in the chemical reaction process can be filtered smoothly, the turbidity of filtrate is reduced to＜10PPM.Be expected to carry out industrial application.
Description of drawings
Fig. 1 is that lime carbonate turbidity and absorbancy concern canonical plotting.
Embodiment
The present invention is further elaborated below by embodiment, but do not limit protection scope of the present invention.
Embodiment 1
Get about 20 ~ 23 grams of 100 ~ 200 purpose alumina powders, kaolin 8 ~ 9 grams, Feldspar Powder 20 ~ 22 grams, add 5 ~ 8 gram ethanolic solns and make defoamer, add 55 ~ 60 gram water earlier and stir, add about 0.3% polyacrylamide solution of about 100 grams then while stirring, make it flocculation sediment.And continue to stir 5 ~ 6 minutes.
Get four parts of powders ready by above proportioning, change rotating speed, get 200 rev/mins, 300 rev/mins, 400 rev/mins and 600 rev/mins respectively.Flocculation, moulding and sintering are made sample.
Sintering: the sintering program is as follows
80～500℃ 105min
500 ℃ of insulation 30min
500～950℃ 45min
950 ℃ of insulation 60min
950～1200℃ 25min
1200 ℃ of insulation 120min
The porosity of each sample is as shown in table 1 respectively:
The relation of table 1 porosity and stir speed (S.S.)
| Stir speed (S.S.) (rev/min) | 200 | 300 | 400 | 600 |
| Porosity (%) | 57.19 | 55.94 | 55.87 | 53.83 |
Along with the increase of stir speed (S.S.), porosity reduces.This is because under the stirring of more speed, shearing force is bigger, and the initial flocculation particle is constantly smashed, and diameter diminishes, thereby porosity constantly reduces.
Embodiment 2
Get about 20 ~ 23 grams of 100 ~ 200 purpose alumina powders, kaolin 8 ~ 9 grams, Feldspar Powder 20 ~ 22 grams, add 5 ~ 8 gram ethanolic solns and make defoamer, add 55 ~ 60 gram water earlier and stir, add about 0.3% polyacrylamide solution of about 100 grams then while stirring, make it flocculation sediment.And continue to stir 5 ~ 6 minutes.Moulding, drying, sintering are made the 1# sample.
Other gets about 20 ~ 23 grams of 200 ~ 300 purpose alumina powders, kaolin 8 ~ 9 grams, Feldspar Powder 20 ~ 22 grams, add 5 ~ 8 gram ethanolic solns and make defoamer, add 55 ~ 60 gram water earlier and stir, add about 0.3% polyacrylamide solution of about 100 grams then while stirring, make it flocculation sediment.And continue to stir 5 ~ 6 minutes.Moulding, drying, sintering are made the 2# sample.Sintering, the sintering program is with embodiment 1
1# and 2# sample are made strainer, and being used for solid-to-liquid ratio is 5: 100 the calcium carbonate superfine powder and the mixed solution of water.
The filtration experiment process: the strainer that uses 1# and 2# sample to make respectively filters solid-to-liquid ratio under the pressure about 0.06MP be 5: 100 the calcium carbonate superfine powder and the mixed solution of water, and obtaining 200 gram filtrates with filtration serves as to filter finish-time.
Sampling: it is the 1-1# sample liquid that the 1# sample filter filters the 200 gram filtrates obtain, filters that to obtain continuing to filter about 40 ~ 50 gram filtrates after the 200 gram filtrates be the 1-2# sample liquid.It is the 2-1# sample liquid that the 2# sample filter filters the 200 gram filtrates obtain, filters that to obtain continuing to filter about 40 ~ 50 gram filtrates after the 200 gram filtrates be the 2-2# sample liquid.
Analyze: use the absorbancy of ultraviolet spectrophotometer at visible region analysis and filter liquid, the sample absorbancy sees Table 2.The standard turbidity curve (Fig. 1) of the mixed solution by calcium carbonate superfine powder and water is analyzed, and draws the turbidity of filtered liquid.With the absorbancy of filtered liquid by with the typical curve analysis of Fig. 1, obtain the turbidity of each sample.
Table 2 sample absorbancy and corresponding turbidimeter
| Sample number | 1-1# | 1-2# | 2-1# | 2-2# |
| Absorbancy | 0.186 | 0.014 | 0.038 | 0.012 |
| The turbidity of absorbancy correspondence (PPM) | 121 | 4 | 23 | 3 |
As seen from Table 2, reduce the granularity of the composition in the ceramic proportioning powder, can prepare hole porous ceramics more uniformly, in the actual filtration application process, can reach the effect that reduces the filtered liquid turbidity by flocculence.
Clear water transmitance value before filtering is 0.314mls
-1Cm
-2, after this, the hydrochloric acid backwash of using 4wt%0.01MP after each the filtration is about 3 minutes, and the clear water transmitance all can be returned to 0.220mls
-1Cm
-2About, it is considerable that as seen it replys efficient.
Embodiment 3
Get about 20 ~ 23 grams of 200 ~ 300 purpose alumina powders, kaolin 8 ~ 9 grams, Feldspar Powder 20 ~ 22 grams, add 5 ~ 8 gram ethanolic solns and make defoamer, add 55 ~ 60 gram water earlier and stir, add about 0.3% polyacrylamide solution of about 100 grams then while stirring, make it flocculation sediment.Stir about adds rapidly 30% Al (H of 5 ~ 8 grams after 3 ~ 5 minutes
2PO
4)
3Solution, restir about 10 seconds immediately.Sintering, the sintering program is with embodiment 1.
The bubble of generation is unlikely to this method because secular stirring and fragmentation, the voidage height of the porous ceramics that the hole of the porous ceramics of making can prepare than flocculence only, and its mean porosities can reach about 59%.
Claims (6)
1, a kind of preparation method of porous ceramics is characterized in that, described method comprises the steps:
1) gets powder: aluminum oxide 20～23 grams, kaolin 8～9 grams, Feldspar Powder 20～22 grams; Add 5～8 gram ethanolic solns and make defoamer;
2, add suitable quantity of water earlier and stir, add the mass ratio be no less than 50g then while stirring and be 0.1%～1% polyacrylamide solution, make it flocculation sediment;
3) continue to stir 5～6 minutes, the speed of stirring is 200～600 commentaries on classics/min;
4) after moulding, drying, sintering program, make porous ceramics.
2, the preparation method of porous ceramics as claimed in claim 1 is characterized in that, described method steps 1) powder in increase a small amount of calcium carbonate powders; The step 3) of described method is: behind the flocculation sediment, stir certain hour, add mass ratio then rapidly and be 5%～35% Al (H
2PO
4)
3The aqueous solution 5～10g continues to stir again, and churning time was no more than for 20 seconds.
3, the preparation method of porous ceramics as claimed in claim 1 or 2 is characterized in that, described powder is 100～300 orders.
4, the preparation method of porous ceramics as claimed in claim 1 or 2 is characterized in that, described sintering program is as follows, and sintering temperature and time are:
80～500℃ 105min
500 ℃ of insulation 30min
500～950℃ 45min
950 ℃ of insulation 60min
950～1200℃ 25min
1200 ℃ of insulation 120min.
5, the preparation method of porous ceramics as claimed in claim 1 is characterized in that, the mass ratio of described polyacrylamide solution is 0.3%.
6, the preparation method of porous ceramics as claimed in claim 2 is characterized in that, in the step 3) of described method, the adding mass ratio is 30% Al (H
2PO
4)
3The aqueous solution 5～8g continues to stir again, and churning time was 10 seconds.
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| CNB2005100270872A CN100334041C (en) | 2005-06-23 | 2005-06-23 | Porous ceramics preparation method |
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| CNB2005100270872A CN100334041C (en) | 2005-06-23 | 2005-06-23 | Porous ceramics preparation method |
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| CN1807355A true CN1807355A (en) | 2006-07-26 |
| CN100334041C CN100334041C (en) | 2007-08-29 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113323B (en) * | 2007-08-02 | 2011-01-19 | 刘光文 | Foam heat storage and method for preparing the same |
| CN101628244B (en) * | 2008-07-16 | 2011-02-09 | 王衍衡 | Process for shaping catalyst into block according to shape of reactor |
| CN101423379B (en) * | 2008-11-12 | 2011-07-06 | 东南大学 | Method for preparing phosphate directional arrangement pore structure porous ceramic |
| CN101423377B (en) * | 2008-11-12 | 2011-07-27 | 东南大学 | Method for preparing directional pore structure phosphate porous ceramic |
| CN101591164B (en) * | 2008-05-30 | 2011-12-28 | 山东理工大学 | Preparation method of porous alumina ceramics |
| CN103342544A (en) * | 2013-07-03 | 2013-10-09 | 镇江市江南矿山机电设备有限公司 | Method for preparing porous alumina ceramic |
| CN105688820A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for processing sludge in urban sewage treatment plant to synthesize mesoporous carbon material through template-like method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6440885B1 (en) * | 1998-12-30 | 2002-08-27 | Corning Incorporated | Zeolite membrane and a process for the production thereof |
| CN1216831C (en) * | 2003-05-14 | 2005-08-31 | 广东省枫溪陶瓷工业研究所 | Making process of porous ceraimc filter element |
-
2005
- 2005-06-23 CN CNB2005100270872A patent/CN100334041C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113323B (en) * | 2007-08-02 | 2011-01-19 | 刘光文 | Foam heat storage and method for preparing the same |
| CN101591164B (en) * | 2008-05-30 | 2011-12-28 | 山东理工大学 | Preparation method of porous alumina ceramics |
| CN101628244B (en) * | 2008-07-16 | 2011-02-09 | 王衍衡 | Process for shaping catalyst into block according to shape of reactor |
| CN101423379B (en) * | 2008-11-12 | 2011-07-06 | 东南大学 | Method for preparing phosphate directional arrangement pore structure porous ceramic |
| CN101423377B (en) * | 2008-11-12 | 2011-07-27 | 东南大学 | Method for preparing directional pore structure phosphate porous ceramic |
| CN103342544A (en) * | 2013-07-03 | 2013-10-09 | 镇江市江南矿山机电设备有限公司 | Method for preparing porous alumina ceramic |
| CN105688820A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for processing sludge in urban sewage treatment plant to synthesize mesoporous carbon material through template-like method |
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|---|---|
| CN100334041C (en) | 2007-08-29 |
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Granted publication date: 20070829 Termination date: 20100623 |