CN100427435C - Method for preparing porous ceramic using modified starch - Google Patents
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- CN100427435C CN100427435C CNB2006101240050A CN200610124005A CN100427435C CN 100427435 C CN100427435 C CN 100427435C CN B2006101240050 A CNB2006101240050 A CN B2006101240050A CN 200610124005 A CN200610124005 A CN 200610124005A CN 100427435 C CN100427435 C CN 100427435C
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- 238000000034 method Methods 0.000 title claims abstract description 11
- 229920000881 Modified starch Polymers 0.000 title claims description 62
- 235000019426 modified starch Nutrition 0.000 title claims description 62
- 239000004368 Modified starch Substances 0.000 title claims description 59
- 229920002472 Starch Polymers 0.000 claims abstract description 88
- 239000008107 starch Substances 0.000 claims abstract description 88
- 235000019698 starch Nutrition 0.000 claims abstract description 88
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000007872 degassing Methods 0.000 claims abstract description 3
- 238000004132 cross linking Methods 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 19
- 125000002091 cationic group Chemical group 0.000 claims description 19
- 239000002131 composite material Substances 0.000 claims description 19
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000006467 substitution reaction Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 15
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- 238000002360 preparation method Methods 0.000 description 5
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- 235000007056 Dioscorea composita Nutrition 0.000 description 4
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- 244000281702 Dioscorea villosa Species 0.000 description 4
- 235000006350 Ipomoea batatas var. batatas Nutrition 0.000 description 4
- 235000004879 dioscorea Nutrition 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
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- 238000012986 modification Methods 0.000 description 4
- 229910052878 cordierite Inorganic materials 0.000 description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 3
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Abstract
The invention discloses a making method of porous ceramic through denaturized starch, which comprises the following steps: mixing alumina and water to prepare ceramic slurry with solid content more than 50vol%; milling to make the ceramic with pH value at 8.0-10.0; degassing; casting in the mould; heating to 60-85 deg.c for 5-60min; sintering; stripping; drying; obtaining the product.
Description
Technical field
The invention belongs to the ceramic material technical field, particularly a kind of method of utilizing modified starch to prepare porous ceramics.
Background technology
Perviousness height, specific surface area are big owing to having for porous ceramics, low density, low-thermal conductivity and advantage such as high temperature resistant, corrosion-resistant are widely used and fields such as chemical industry, environmental protection, the energy, metallurgy, electronics.In recent years, the Application Areas of porous ceramics expands to fields such as aviation again, and the widespread use of porous ceramics has caused the great attention of global material circle.
In the prior art, in order to obtain high performance porous ceramics, people organically combine the moulding and the pore technology of porous ceramics, have developed the novel process of a series of preparation porous ceramicss.The natural macromolecule amylose gel casting forming has converged the advantage of directly solidifying casting (DCC) and gel casting forming (Gel-casting) technology, has overcome their weak point simultaneously, is a kind of rising new technology of ceramic moulding.Yet most of natural polysaccharide has extremely strong water-soluble, meets water dissolution and forms liquid of vicidity, is unfavorable for the moulding of porous ceramics, must add pore-creating agent and could form and have definite shape and big or small opening structure.And gelatinization takes place during its aqueous dispersions heating to form gel in starch and the same natural polysaccharides that belong to together such as agarose, gelatin, and cold water is insoluble, the peculiar property of expanded by heating but starch granules has, and this is highly beneficial to forming the controlled vesicular structure of hole dimension.H.M.Alves etc. are at " utilizing starch to solidify the preparation porous cordierite ceramics " [H.M.Alves, G.Tar í, A.T.Fonseca, J.M.F.Ferreira.Processingof porous cordierite bodies by starch consolidation.Materials Research Bulletin, 1998,33 (10): 1439-1448] in the literary composition, starch is made solidifying agent and pore former successfully molds porous cordierite ceramics.M.E.Bowden etc. are at " utilizing starch coagulation forming porous ceramics " [M.E.Bowden, M.S.Rippey.Porous ceramics formed using starch consolidation.Key Eng Mater, 2002,206-213:1957-1960] in the literary composition, respectively rice, corn and yam starch are used for the coagulation forming alumina porous ceramic, its porosity is in 15～45% scopes.Porosity is that 40% ceramic intensity is still more than 100MPa.Research shows that also compare with yam starch with corn, the ceramic body aperture of Starch rice moulding is tiny, but corresponding biscuit intensity is low, only is 0.5MPa, and uses W-Gum or yam starch, and the biscuit of ceramics intensity that obtains is 1.5MPa.E.
Deng at " starch solidifies formed alumina ceramic body and microcosmos structure characteristic " [E.
W.Pabst, E.Gregorov á, J.Havrda.Starch consolidation casting of alumina ceramics-Body formation andmicrostructural characterization.Key Eng Mater, 2002,206-213:1969-1972] in the literary composition, with consumption is that 5～30% yam starch is cured the formed alumina porous ceramics, and the density that obtains base substrate is 3.31～2.51g/cm
3, the base substrate linear shrinkage ratio is between 13～16% behind the sintering, and the goods porosity is 17～37%.Though different types of ative starch has different separately structural performances, porous ceramic film material requires very high for opening structure, size, distribution, and this is the critical problem that present ative starch cann't be solved.
Summary of the invention
In order to overcome the shortcoming that existing starch consolidation in-situ forming prepares the porous ceramics technology, the object of the present invention is to provide that a kind of technology is simple, the accurate porous ceramics preparation method of control of opening structure, size, this method prepares porous ceramics with modified starch or composite modified starch as the solidifying agent of pore-creating agent and consolidation in-situ forming, when reaching porous ceramics opening structure and the accurate control of size by adjusting to modified starch or composite modified starch expansion character, realize the near-net-shape of pottery, thereby significantly improve the performance of porous ceramics.
Purpose of the present invention is achieved through the following technical solutions: a kind of method of utilizing modified starch to prepare porous ceramics comprises the steps:
Aluminum oxide powder and water are mixed with the ceramic size of solid content greater than 50vol%, in ceramic size, add modified starch according to the ratio of aluminum oxide powder 30～50vol%, after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size, after the degassing ceramic size is injected mould, be heated to 60～85 ℃, be incubated 5～60 minutes; The dried ceramic body of the demoulding gets goods behind sintering.
In order to realize the present invention better, described modified starch comprises the composite modified starch of any modified starch in Sumstar 190, acetate starch, cross-linking starch, cationic starch, high chain starch and Sumstar 190 or acetate starch or cross-linking starch or the cationic starch or the composite modified starch of any modified starch in cross-linking starch and Sumstar 190 or acetate starch or the cationic starch.
The mobility of described Sumstar 190 is 30～80; The substitution value of acetate starch is 0.002～2.68; The degree of crosslinking of cross-linking starch is 4.37 * 10
-2～6.0 * 10
-2The cationic starch substitution value is 0.01～0.5; The chain starch content scope of high chain starch is 50～80%
The ratio of any modified starch in the described composite modified starch in high chain starch and Sumstar 190 or acetate starch or cross-linking starch or the cationic starch: any modified starch in Sumstar 190 or acetate starch or cross-linking starch or the cationic starch accounts for 0.1～10% by weight percentage, and high chain starch accounts for 90～99.9% by weight percentage.
The ratio of any modified starch in the described composite modified starch in cross-linking starch and Sumstar 190 or acetate starch or the cationic starch: any modified starch in Sumstar 190 or acetate starch or the cationic starch accounts for 0.1～10% by weight percentage, and cross-linking starch accounts for 90～99.9% by weight percentage.
The present invention compared with prior art has following advantage and beneficial effect:
1, the present invention utilizes modified starch particulate swelling character cleverly, first with its consolidation in-situ forming solidifying agent and pore former as porous ceramics, the moulding and the pore technology of porous ceramics slurry can organically be combined, thereby set up a kind of multi-functional efficient, low-cost, simple porous ceramics new preparation technology of technology.
2, the present invention is under the prerequisite that guarantees ceramic size high quality consolidation in-situ forming, utilize the modification degree and the modification mode of regulating modified starch can control the expansion behavior of particle in ceramic size, thereby obtain satisfied pore size, distribution and hole rate 40～80%.But also can select the modified starch synergy of different expansion behaviors for use, and prepare oxide porous ceramic with hole gradient, have the better application prospect.
3, the modified starch ash oontent is low, be subjected to can not constitute pollution to product in the thermal process at ceramic body, and mainly be carbonic acid gas and water vapor because of the gas of emitting simultaneously, pollution-free substantially to environment.
4, extensive, the low price of starch source, modified starch is of a great variety, because ative starch is by after physics, chemistry and the biotechnology modification, give the physicochemical property that it was not had originally, make its application widely that obtained, as fields such as food, weaving, papermaking, derived energy chemicals at industrial circle.It is applied to prepare porous ceramics and compares with other preparation methods, have renewable, production cost is low, the advantages such as application that can be mass-produced will produce good social benefit and economic benefit.
Description of drawings
Fig. 1 is one scan electron microscope (SEM) photo of the embodiment of the invention four goods sections.
Fig. 2 is one scan electron microscope (SEM) photo of the embodiment of the invention four goods sections.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment one: modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 58vol%.Add modified starch according to the ratio of aluminum oxide powder 30vol%, after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, be heated to 60 ℃, be incubated and take out cooling after 1 hour.The dried ceramic body of the demoulding gets goods behind sintering.Porosity, the ultimate compression strength of resulting product are as shown in table 1.
Table 1
Embodiment two: modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 55vol%.Add modified starch according to the ratio of aluminum oxide powder 40vol%, after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, be heated to 60 ℃, be incubated and take out cooling after 1 hour.The dried ceramic body of the demoulding gets goods behind sintering.Porosity, the ultimate compression strength of resulting product are as shown in table 2.
Table 2
Embodiment three: modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 58vol%.Add modified starch according to the ratio of aluminum oxide powder 50vol%, after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, be heated to 80 ℃, be incubated and take out cooling after 45 minutes.The dried ceramic body of the demoulding gets goods behind sintering.Porosity, the ultimate compression strength of resulting product are as shown in table 3.
Table 3
Embodiment four: modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 58vol%.Add modified starch according to the ratio of aluminum oxide powder 50vol%, after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, be heated to 85 ℃, be incubated and take out cooling after 5 minutes.The dried ceramic body of the demoulding gets goods behind sintering.As depicted in figs. 1 and 2, be scanning electronic microscope (SEM) photo of said products section.Wherein Fig. 1 amplifies 500 times cross-section morphology photo, and the almost spherical macropore is formed by modified starch among Fig. 1.Fig. 2 amplifies 2000 times cross-section morphology photo, and it is many by the macropore that forms after the calcination of modified starch particle to distribute in the visual field as can be seen, and aperture size is between 4～10 μ m.Porosity, the ultimate compression strength of resulting product are as shown in table 4.
Table 4
Embodiment five: composite modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 58vol%.Ratio according to aluminum oxide powder 50vol% adds composite modified starch, and the ratio of any modified starch of wherein high chain starch and Sumstar 190 or acetate starch or cross-linking starch or cationic starch sees Table 5-1,5-2,5-3.The alumina-ceramic slurry that adds different composite modified starches is after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, take out cooling by the condition heating shown in table 5-1,5-2, the 5-3, insulation back.The dried ceramic body of the demoulding gets goods behind sintering.The porosity of resulting product, ultimate compression strength are shown in table 5-1,5-2,5-3.
Table 5-1
Table 5-2
Table 5-3
Embodiment six: composite modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 58vol%.Ratio according to aluminum oxide powder 50vol% adds composite modified starch, and wherein the ratio of any modified starch of cross-linking starch and Sumstar 190 or acetate starch or cationic starch sees Table 6-1,6-2,6-3.The alumina-ceramic slurry that adds different composite modified starches is after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, take out cooling by the condition heating shown in table 6-1,6-2, the 6-3, insulation back.The dried ceramic body of the demoulding gets goods behind sintering.The porosity of resulting product, ultimate compression strength are shown in table 6-1,6-2,6-3.
Table 6-1
Table 6-2
Table 6-3
Embodiment seven: composite modified starch prepares alumina porous ceramic
(median size 0.3 μ m) mixes with water aluminum oxide powder, is prepared into the ceramic size that solid content is 50vol%.Ratio according to aluminum oxide powder 40vol% adds composite modified starch, and wherein the ratio of any modified starch of cross-linking starch and Sumstar 190 or acetate starch or cationic starch sees Table 7.The alumina-ceramic slurry that adds different composite modified starches is after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size.After the vacuum outgas ceramic size is injected metal die, press the condition heating shown in the table 7, the taking-up cooling of insulation back.The dried ceramic body of the demoulding gets goods behind sintering.Porosity, the ultimate compression strength of resulting product are as shown in table 7.
Table 7
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (3)
1, a kind of method of utilizing modified starch to prepare porous ceramics is characterized in that comprising the steps:
Aluminum oxide powder and water are mixed with the ceramic size of solid content greater than 50vol%, in ceramic size, add modified starch according to the ratio of aluminum oxide powder 30～50vol%, after ball milling mixes and to make the pH value be 8.0～10.0 ceramic size, after the degassing ceramic size is injected mould, be heated to 60～85 ℃, be incubated 5～60 minutes; The dried ceramic body of the demoulding obtains goods behind sintering;
Described modified starch comprises the composite modified starch of any modified starch in Sumstar 190, acetate starch, cross-linking starch, cationic starch, high chain starch and Sumstar 190 or acetate starch or cross-linking starch or the cationic starch or the composite modified starch of any modified starch in cross-linking starch and Sumstar 190 or acetate starch or the cationic starch;
The mobility of described Sumstar 190 is 30～80; The substitution value of acetate starch is 0.002～2.68; The degree of crosslinking of cross-linking starch is 4.37 * 10
-2～6.0 * 10
-2The cationic starch substitution value is 0.01～0.5; The chain starch content scope of high chain starch is 50～80%.
2, a kind of method of utilizing modified starch to prepare porous ceramics according to claim 1, it is characterized in that: the ratio of any modified starch in the described composite modified starch in high chain starch and Sumstar 190 or acetate starch or cross-linking starch or the cationic starch: any modified starch in Sumstar 190 or acetate starch or cross-linking starch or the cationic starch accounts for 0.1～10% by weight percentage, and high chain starch accounts for 90～99.9% by weight percentage.
3, a kind of method of utilizing modified starch to prepare porous ceramics according to claim 1, it is characterized in that: the ratio of any modified starch in the described composite modified starch in cross-linking starch and Sumstar 190 or acetate starch or the cationic starch: any modified starch in Sumstar 190 or acetate starch or the cationic starch accounts for 0.1～10% by weight percentage, and cross-linking starch accounts for 90～99.9% by weight percentage.
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| CN102617154B (en) * | 2012-04-01 | 2014-10-01 | 景德镇陶瓷学院 | Method for preparing environment-friendly building ceramic tile by using high lean material |
| CN104108948A (en) * | 2013-04-22 | 2014-10-22 | 中微半导体设备(上海)有限公司 | Method for preparing semiconductor reaction chamber component and component |
| CN103951462B (en) * | 2014-04-28 | 2015-06-03 | 胡海波 | Preparation method of high-strength light-weight ceramic plate |
| CN104446625A (en) * | 2014-11-28 | 2015-03-25 | 中国科学技术大学先进技术研究院 | High-porosity porous ceramic and preparation method thereof |
| CN108675823A (en) * | 2018-04-20 | 2018-10-19 | 安徽中都环宇新材料科技有限公司 | A kind of diesel emission particulate purification DPF honeycomb ceramic carriers |
| CN112577851A (en) * | 2020-11-23 | 2021-03-30 | 龙岩高岭土股份有限公司 | Method for improving plasticity of ceramic raw material |
| CN114933486B (en) * | 2022-04-28 | 2023-07-28 | 辽宁大学 | Method for preparing porous ceramic block body based on water-based slurry through 3D printing |
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Non-Patent Citations (6)
| Title |
|---|
| Processing of Porous Ceramics by ‘Starch Consolidation’. O. Lyckfeldt, J. M. F. Ferreirab.Journal of European Ceramic Society,Vol.18 . 1998 |
| Processing of Porous Ceramics by ‘Starch Consolidation’. O. Lyckfeldt, J. M. F. Ferreirab.Journal of European Ceramic Society,Vol.18 . 1998 * |
| 变性淀粉取代聚乙烯醇生产Al2O3刚玉陶瓷的胶年剂研究. 周小明，刘卫东.中国陶瓷工业，第10卷第3期. 2003 |
| 变性淀粉取代聚乙烯醇生产Al2O3刚玉陶瓷的胶年剂研究. 周小明，刘卫东.中国陶瓷工业，第10卷第3期. 2003 * |
| 淀粉及改性淀粉在高性能陶瓷制备中的应用. 琚晨辉，叶建东，宋贤良，吴彤.材料导报，第1期. 2006 |
| 淀粉及改性淀粉在高性能陶瓷制备中的应用. 琚晨辉，叶建东，宋贤良，吴彤.材料导报，第1期. 2006 * |
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