CN102173852B - Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique - Google Patents
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Abstract
The invention relates to a method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique, which comprises the following steps: (1) by using alkane or ester containing more than four carbon atoms as a disperse phase and using surfactant with an HLB (hydrophile-lipophile balance) value of 8-20 as an emulsifier, stirring to obtain an oil-in-water emulsion; (2) preparing a stable suspension containing organic monomers, a crosslinking agent, a catalyst, a dispersant and ceramic powder; (3) mixing the emulsion and suspension to obtain a slurry, adding a proper amount of initiator, and evenly stirring; (4) casting the slurry into a die, carrying out crosslinking curing, stripping, drying the blank, and discharging adhesive from the blank; and (5) sintering the blank by using a certain firing procedure, thereby finally obtaining the alumina porous ceramics. The number and size of pores of the porous ceramics can be effectively regulated and controlled, the required device and technological process are simple, and the porous ceramics have high mechanical strength.
Description
Technical field
The present invention relates to a kind of method of preparing alumina porous ceramics by emulsion/gel-combined die casting technique, relate to or rather a kind of with the approach of the oil droplet in the oil-in-water emulsion as the introducing pore, and the preparation light porous heat-insulating material that combines with the aqueous gelcasting mold technique, belong to the porous ceramics field.
Background technology
Porous ceramics has the advantages such as porosity is high, density is low, high temperature resistant, corrosion-resistant, all has broad application prospects in fields such as metallurgy, catalysis, chemical industry, environmental protection, the energy.At present, the preparation method of porous ceramics mainly contains and adds solid pore-forming material method, foaming, organic precursor pickling process etc.Solid pore-forming material method is by adding solid pore-forming material (such as graphite, starch, sawdust etc.) when the ceramic batch, occupy certain space in ceramic body, in sintering process pore-forming material is burnt and forms pore.The porous ceramics air hole structure of this method preparation is different, and void content is lower and gas cell distribution is inhomogeneous.Foaming is to add organic or inorganic foaming agent in ceramic size, produces foam in whipping process, and drying and sintering make porous ceramics.The standby porous ceramics aperture of this legal system is less and mostly be the hole of holding one's breath, but foaming is to the having relatively high expectations of raw material, and processing condition are wayward.Organic precursor pickling process is mainly for the preparation of the perforate porous ceramics, and the tridimensional network that utilizes Organic Foam Material (such as polyurethane sponge etc.) to have evenly is coated in slurry on the Organic Foam Material, obtains netted porous ceramics after burning foams.The porous ceramics void content of this technique preparation is higher, and the aperture is large, is mainly used in melted metal filter.
Milk sap refers to that a kind of liquid is dispersed in another kind of and its not miscible liquid and the dispersion system that forms with the form of drop.Drop is called disperse phase, and the liquid of another kind of continuous distribution is called dispersion medium.Milk sap can be divided into two types of oil-in-water (oil-in-water, O/W) and water-in-oils (water-in-oil, W/O) usually.The preparation of true emulsion need to add certain tensio-active agent, i.e. emulsifying agent usually.Adjust the ratio of water, oil and emulsifying agent, can make the size of disperse phase less than 100nm, at this moment milk sap becomes transparent, and more stable, is called microemulsion.At present, Water in Oil emulsion has been widely used in the especially preparation of nanometer grade powder of inorganic materials superfine powder, and oil-in-water emulsion then is mainly used in pharmaceutical carrier and pesticide field.Oil phase in the oil-in-water emulsion as pore-forming material, is expected to the preparation for porous ceramic film material, and its precondition is that the oil droplet original position of will disperse is fixed in the ceramic body.
In the invention nineties in 20th century, it combines traditional slip-casting shaping process and organic chemistry macromolecular polymerization reaction gel injection molding and forming technology dexterously by U.S. Oak Ridge National Key Laboratory, can be used for the material preparation of different shape complexity.The ultimate principle of this technique is by preparation high solid loading, low viscous ceramic size, again by adding a small amount of initiator and catalyzer or making organic monomer and linking agent polymerization reaction take place in the slurry make the slurry in-situ solidifying by the mode that heats, obtain the base substrate of high strength, good uniformity, then through operations such as super-dry, binder removal and sintering, prepare the ceramic component of near net-shape.This forming technique has received various countries scientific worker's concern since invention, especially have larger advantage when the ceramic part of moulding complicated shape.
Adopt water system gel injection technique, just the oil phase drop original position in the oil-in-water emulsion can be fixed in the base substrate of curing, and ceramic powder and gelling system still are distributed in aqueous phase.This is equivalent to add the drop pore-forming material in ceramic size, successfully introduces pore thereby in sintering process the oil phase drop burnt.By a large amount of literature searches, do not find that the method that adopts milk sap to combine with gel injection molding and forming technology prepares the report of porous ceramics.
Summary of the invention
The object of the invention is to propose a kind of method of preparing alumina porous ceramics by emulsion/gel-combined die casting technique, oil-in-water emulsion is combined with gel injection technique, realize the pore quantity of porous ceramic film material and regulating and control of size, the porous ceramics that makes simultaneously possesses higher physical strength.
The technical scheme that the present invention proposes is: a kind of method of preparing alumina porous ceramics by emulsion/gel-combined die casting technique, described preparation method comprise drying, binder removal and the sintering of base substrate behind the mixed gel casting forming of preparation, milk sap and suspension, moulding of the ceramic powder stable suspension of the preparation of oil-in-water emulsion, certain solid load.Its concrete processing step is:
1) preparation of oil-in-water emulsion:
Take water as dispersion medium, take the organism of 0.5～10 times of volume of dispersion medium as disperse phase, and add HLB value at 8～20 tensio-active agent as emulsifying agent, prepare the oil-in-water-type true emulsion through stirring.Wherein, described organism is to contain four carbon atom above alkane or ester class, described tensio-active agent is a kind of in anion surfactant, cats product, the nonionogenic tenside, and its consumption is the disperse phase quality
2) have the preparation of the ceramic powder stable suspension of certain solid load:
With water, organic monomer, linking agent, catalyzer, dispersion agent and alumina powder jointed the batching, and carry out ball milling and mix, obtain solid load at 20～80% stable suspension.Wherein, described organic monomer is a kind of in acrylamide AM, Methacrylamide MAM, propyl group acrylamide, vinyl pyrrolidone NVP, β-dimethyl-aminoethylmethacrylate, the vinylbenzene; Described linking agent is a kind of in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA, the propenyl methyl acrylate; Described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine TEMED; Described dispersion agent is a kind of in tripolyphosphate ammonium, Hexamethylphosphoric acid triamide, the ammonium polyacrylate; The consumption of dispersion agent, organic monomer, linking agent, catalyzer is respectively 0.1～3.0%, 3～10%, 0.1～2.0%, 0.01～0.3% of aluminum oxide powder weight; Described ball milling hybrid technique, ball milling speed are 20～300r/min, and Ball-milling Time is 0.5～12h;
3) the mixed gel casting forming of milk sap and suspension:
With milk sap and suspension mix and blend and add initiator, be stirred well to evenly, then mixed slurry is injected the mould of smearing releasing agent and make it that crosslinking reaction occur, carry out the demoulding after leaving standstill for some time.Wherein, the volume ratio of milk sap and suspension is 1: 4～8: 1; Described initiator is persulphate, and consumption is 10～80% of monomer mass, and described crosslinking time is 1～30min;
4) drying of base substrate, binder removal and sintering:
Base substrate after the demoulding is successively carried out drying in climatic chamber and common loft drier; Then in air atmosphere, carry out binder removal and sintering.Described climatic chamber is dry, and temperature and humidity is respectively at 35～80 ℃, 30～90%, and the time length is 4～12h; Described common loft drier is dry, and temperature is at 80～110 ℃, and the time length is 6～36h; Described binder removal, temperature rise rate are 0.3～1 ℃/min, and in 300～600 ℃ of insulation 0.5～5h; Described sintering process, temperature rise rate are 0.5～3 ℃/min, and in 1400～1700 ℃ of insulation 1～3h.
Organism as disperse phase can be: a kind of in pentamethylene, hexanaphthene, normal heptane, octane, isopropyl laurate, ethyl palmitate, the n-capric acid methyl esters.
Tensio-active agent as emulsifying agent can be: a kind of in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, cetyl trimethylammonium bromide, the tween series of surfactants.
Persulphate as initiator can be: a kind of in Sodium Persulfate, Potassium Persulphate, the ammonium persulphate.
Advantage of the present invention:
Oil-in-water emulsion is combined with gel injection technique, can realize the pore quantity of porous ceramic film material and the regulation and control of size by the adjusting to the milk sap proportion of composing, required equipment and technical process are fairly simple, applicable ceramic systems is wide, and prepared finished product has higher physical strength simultaneously.
Description of drawings
Fig. 1 is the electron scanning micrograph of the embodiment of the invention 1 prepared sample section.
Embodiment
Embodiment 1
At first take water as dispersion medium, take pentamethylene as disperse phase, take cetyl trimethylammonium bromide as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 3 times of water, emulsifier is going of disperse phase quality.Take Hexamethylphosphoric acid triamide as dispersion agent, acrylamide is monomer, methylene-bisacrylamide is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 12h of 20r/min, the preparation solid load is 70% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 1.0%, 8.0%, 2.0%, 0.05% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 1: 1 and add ammonium persulphate as initiator, consumption is 10% of monomer mass, and the rear injection mould that stirs leaves standstill 30min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 40 ℃ and 40%, and then insulation 6h changes in 100 ℃ the common loft drier and be incubated 6h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 0.5 ℃/min rise to 400 ℃ of insulation 3h, to remove organism wherein, then rise to 1600 ℃ and be incubated 1h with the temperature rise rate of 1 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 58%, and ultimate compression strength is 25MPa.Fig. 1 has provided the microtexture of section hole behind the porous ceramics sintering.
Embodiment 2
At first take water as dispersion medium, take normal heptane as disperse phase, take Sodium dodecylbenzene sulfonate as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 10 times of water, emulsifier is the disperse phase quality
Take ammonium polyacrylate as dispersion agent, Methacrylamide is monomer, diallyl tartrate diamide is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 8h of 50r/min, the preparation solid load is 80% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 3.0%, 4.0%, 0.8%, 0.01% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 8: 1 and add Sodium Persulfate as initiator, consumption is 30% of monomer mass, and the rear injection mould that stirs leaves standstill 10min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 60 ℃ and 50%, and then insulation 8h changes in 90 ℃ the common loft drier and be incubated 24h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 0.3 ℃/min rise to 400 ℃ of insulation 4h, to remove organism wherein, then rise to 1400 ℃ and be incubated 1h with the temperature rise rate of 0.5 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 85%, and ultimate compression strength is 15MPa.
Embodiment 3
At first take water as dispersion medium, take octane as disperse phase, take sodium lauryl sulphate as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 5 times of water, emulsifier is the disperse phase quality
Take the tripolyphosphate ammonium as dispersion agent, vinyl pyrrolidone is monomer, methylene-bisacrylamide is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 4h of 100r/min, the preparation solid load is 60% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 0.1%, 3%, 0.1%, 0.1% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 4: 1 and add Potassium Persulphate as initiator, consumption is 60% of monomer mass, and the rear injection mould that stirs leaves standstill 5min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 55 ℃ and 80%, and then insulation 10h changes in 110 ℃ the common loft drier and be incubated 10h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 0.8 ℃/min rise to 300 ℃ of insulation 5h, to remove organism wherein, then rise to 1500 ℃ and be incubated 3h with the temperature rise rate of 3 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 51%, and ultimate compression strength is 27MPa.
Embodiment 4
At first take water as dispersion medium, take isopropyl laurate as disperse phase, take tween 80 as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 7 times of water, emulsifier is the disperse phase quality
Take Hexamethylphosphoric acid triamide as dispersion agent, acrylamide is monomer, the propenyl methyl acrylate is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 1h of 200r/min, the preparation solid load is 62% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 0.5%, 10%, 1.2%, 0.2% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 2: 1 and add Sodium Persulfate as initiator, consumption is 30% of monomer mass, and the rear injection mould that stirs leaves standstill 15min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 35 ℃ and 90%, and then insulation 12h changes in 100 ℃ the common loft drier and be incubated 30h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 1 ℃/min rise to 600 ℃ of insulation 0.5h, to remove organism wherein, then rise to 1700 ℃ and be incubated 1h with the temperature rise rate of 2 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 70%, and ultimate compression strength is 18MPa.
Embodiment 5
At first take water as dispersion medium, take ethyl palmitate as disperse phase, take polysorbate60 as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 0.5 times of water, emulsifier is the disperse phase quality
Take ammonium polyacrylate as dispersion agent, β-dimethyl-aminoethylmethacrylate is monomer, methylene-bisacrylamide is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 0.5h of 300r/min, the preparation solid load is 30% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 1.5%, 7%, 1.5%, 0.12% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 1: 4 and add ammonium persulphate as initiator, consumption is 80% of monomer mass, and the rear injection mould that stirs leaves standstill 1min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 80 ℃ and 70%, and then insulation 4h changes in 110 ℃ the common loft drier and be incubated 6h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 0.5 ℃/min rise to 300 ℃ of insulation 3h, to remove organism wherein, then rise to 1650 ℃ and be incubated 2h with the temperature rise rate of 2 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 25%, and ultimate compression strength is 103MPa.
Embodiment 6
At first take water as dispersion medium, take the n-capric acid methyl esters as disperse phase, take cetyl trimethylammonium bromide as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 2 times of water, emulsifier is the disperse phase quality
Take the tripolyphosphate ammonium as dispersion agent, acrylamide is monomer, the propenyl methyl acrylate is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 6h of 150r/min, the preparation solid load is 20% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 2.0%, 5%, 1.0%, 0.3% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 1: 2 and add ammonium persulphate as initiator, consumption is 50% of monomer mass, and the rear injection mould that stirs leaves standstill 20min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 70 ℃ and 60%, and then insulation 7h changes in 80 ℃ the common loft drier and be incubated 36h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 0.7 ℃/min rise to 500 ℃ of insulation 4h, to remove organism wherein, then rise to 1550 ℃ and be incubated 2h with the temperature rise rate of 1 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 45%, and ultimate compression strength is 82MPa.
Embodiment 7
At first take water as dispersion medium, take hexanaphthene as disperse phase, take sodium lauryl sulphate as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 6 times of water, emulsifier is the disperse phase quality
Take ammonium polyacrylate as dispersion agent, the propyl group acrylamide is monomer, methylene-bisacrylamide is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 2h of 80r/min, the preparation solid load is 50% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 0.3%, 9%, 0.5%, 0.08% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 5: 1 and add Potassium Persulphate as initiator, consumption is 40% of monomer mass, and the rear injection mould that stirs leaves standstill 3min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 60 ℃ and 70%, and then insulation 6h changes in 100 ℃ the common loft drier and be incubated 20h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 1 ℃/min rise to 400 ℃ of insulation 5h, to remove organism wherein, then rise to 1450 ℃ and be incubated 1h with the temperature rise rate of 2 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 68%, and ultimate compression strength is 18MPa.
Embodiment 8
At first take water as dispersion medium, take ethyl palmitate as disperse phase, take Sodium dodecylbenzene sulfonate as emulsifying agent, preparation milk sap, wherein the disperse phase volume is 4 times of water, emulsifier is the disperse phase quality
Take the tripolyphosphate ammonium as dispersion agent, vinylbenzene is monomer, diallyl tartrate diamide is linking agent, N, N, N ', N '-Tetramethyl Ethylene Diamine is catalyzer, with the rotating speed planetary ball mill 2h of 100r/min, the preparation solid load is 55% alumina stable suspension, and wherein the consumption of dispersion agent, monomer, linking agent, catalyzer is respectively 1.0%, 6%, 1.4%, 0.15% of quality of alumina.Milk sap and suspension are mixed with volume ratio at 3: 1 and add ammonium persulphate as initiator, consumption is 20% of monomer mass, and the rear injection mould that stirs leaves standstill 10min, the demoulding.Base substrate after the demoulding places climatic chamber, and temperature humidity is respectively 75 ℃ and 80%, and then insulation 8h changes in 105 ℃ the common loft drier and be incubated 12h.Base substrate after the oven dry first in tube furnace the temperature rise rate with 0.5 ℃/min rise to 500 ℃ of insulation 2h, to remove organism wherein, then rise to 1550 ℃ and be incubated 2h with the temperature rise rate of 1.5 ℃/min, burn till porous ceramics.The porosity of gained porous ceramics is 55%, and ultimate compression strength is 26MPa.
Claims (11)
1. the method for a preparing alumina porous ceramics by emulsion/gel-combined die casting technique is characterized in that: described preparation method comprises drying, binder removal and the sintering of base substrate behind the mixed gel casting forming of preparation, milk sap and suspension, moulding of the ceramic powder stable suspension of the preparation of oil-in-water emulsion, certain solid load;
1) preparation of oil-in-water emulsion:
Take water as dispersion medium, take the organism of 0.5～10 times of volume of dispersion medium as disperse phase, and add the HLB value at 8～20 tensio-active agent as emulsifying agent, the volume of tensio-active agent is disperse phase
Through stirring preparation oil-in-water-type true emulsion;
2) preparation of the ceramic powder stable suspension of certain solid load:
With water, organic monomer, linking agent, catalyzer, dispersion agent and alumina powder jointed the batching, and carry out ball milling and mix, obtain solid load and be 20～80% stable suspension; Dispersion agent, organic monomer, linking agent, catalyst levels are respectively 0.1～3.0%, 3～10%, 0.1～2.0%, 0.01～0.3% of aluminum oxide powder weight;
3) the mixed gel casting forming of milk sap and suspension:
Milk sap and suspension are mixed and add initiator according to a certain volume, be stirred well to evenly, then mixed slurry is injected the mould of smearing releasing agent, carry out the demoulding after leaving standstill for some time;
4) drying of base substrate, binder removal and sintering:
Base substrate after the demoulding is successively carried out drying in climatic chamber and common loft drier; Then in air atmosphere, carry out binder removal and sintering.
2. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, it is characterized in that described organism is to contain four carbon atom above alkane or ester class.
3. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, it is characterized in that described tensio-active agent is a kind of in anion surfactant, cats product, the nonionogenic tenside.
4. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, it is characterized in that described organic monomer is a kind of in acrylamide AM, Methacrylamide MAM, propyl group acrylamide, vinyl pyrrolidone NVP, β-dimethyl-aminoethylmethacrylate, the vinylbenzene; Described linking agent is a kind of in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA or the propenyl methyl acrylate; Described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine TEMED; Described dispersion agent is a kind of in tripolyphosphate ammonium or Hexamethylphosphoric acid triamide or the ammonium polyacrylate.
5. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, it is characterized in that described ball milling hybrid technique, ball milling speed is 20～300r/min, and Ball-milling Time is 0.5～12h.
6. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, it is characterized in that the volume ratio when described milk sap and suspension mix is 1: 4～8: 1; Described initiator is persulphate, and consumption is 10～80% of monomer mass; Described crosslinking time is 1～30min.
7. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, it is characterized in that carrying out dry temperature, humidity at climatic chamber is controlled at respectively 35～80 ℃, 30～90%, the time length is 4～12h; Carry out dry temperature at common loft drier and be controlled at 80～110 ℃, the time length is 6～36h.
8. by the method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique claimed in claim 1, when it is characterized in that the base substrate binder removal, temperature rise rate is 0.3～1 ℃/min, and in 300～600 ℃ of insulation 0.5～5h; Temperature rise rate is 0.5～3 ℃/min during sintering, and in 1400～1700 ℃ of insulation 1～3h.
9. by the method for claim 1 or 2 described preparing alumina porous ceramics by emulsion/gel-combined die casting techniques, it is characterized in that as the organism of disperse phase being: a kind of in pentamethylene, hexanaphthene, normal heptane, octane, isopropyl laurate, ethyl palmitate, the n-capric acid methyl esters.
10. by the method for claim 1 or 3 described preparing alumina porous ceramics by emulsion/gel-combined die casting techniques, it is characterized in that as the tensio-active agent of emulsifying agent being: a kind of in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, cetyl trimethylammonium bromide, the tween series of surfactants.
11. annotate the method that membrane process prepare alumina porous ceramic by claim 1 or 5 described milk sap attached gels, it is characterized in that as the persulphate of initiator being: a kind of in Sodium Persulfate, Potassium Persulphate, the ammonium persulphate.
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