CN1669705A - Porous inorganic microstraining core and preparation method thereof - Google Patents
Porous inorganic microstraining core and preparation method thereof Download PDFInfo
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Abstract
This invention provides an inorganic porous filter element for micro straining and its preparation method, which is characterized by the following steps: a, making out compound base by stirring mixture of base, carrier and firming additive for 2-4 hours, then making out a porous grease by press forming and reaction solidifying; b, demoulding and drying the grease, then sintering it at temperature of 700-1550Deg.C, insulating for 1-2 hours, after cool-down to get filter element. A Wherein, the base is metallic nickel, titanium, stainless steel, bronze, copper powder, monox, alumina, bergmeal, pearlite, quartz sand and cordierite porcelain flour; the carrier is water or alcohol. The method has good pressed intensity, suitable for filter element device of cored, disk-type, bowl-type, hemispherical and bullet-type.
Description
Technical field
The present invention relates to the inorganic functional material field, belong to porous inorganic microstraining core and prepare category, a kind of porous inorganic microstraining core and preparation method thereof is provided.
Background technology
The porous ceramic micro filter filter core has high temperature resistant, corrosion-resistant, capable of washing advantage, and high temperature resistant, characteristics such as intensity is high, easy sealing that the porous metal microstraining core has have purposes widely in industries such as water treatment, environmental protection, food, electric power.
Inorganic porous material mainly contains porous ceramics and porous metal.The general forming methods such as traditional extruding, slip casting that adopt of porous ceramics, in order to obtain suitable aperture and hole, mostly be at high temperature to burn the pore former of mistake by adding, have that green strength is poor, time of drying is long, and the aperture of losing acquisition by the burning of pore former is big, occur defective easily, the lack of homogeneity in hole influences its filter effect.Chinese invention patent " a kind of preparation method of high porosity porous ceramics " (application number 03132960) is with conventional ceramic material technology, added the pore-forming material that reaches 50-80% by weight percentage, and will be with dried ceramic body successively through leaching, drying, dipping sintering aid, drying, operation such as burn till and obtain porous ceramics.The organic foam small-sphere that Chinese invention patent " organic foam small-sphere is as the preparation method of the injection moulding porous ceramics of pore former " (application number 03128065) at first utilizes the paraffin molten immersion treatment to cross, then with ceramic powder and bio-vitric binding agent mixing, hot-injection molding, through dewaxing, plastic removal, sintering processes, obtain product.Chinese invention patent " the water-base gel casting legal system is equipped with the technology of porous ceramics " (application number 03128066) at first will prepare and contain organic monomer, linking agent, initiator, the more stable suspension of dispersion agent and ceramic powder, adding volume fraction again in above-mentioned composite base-material is the surface treated pore-forming material of 50-80% (with respect to above-mentioned suspension vol), add that suitable pressure is in contact with one another pore-forming material and also can be uniformly distributed in the suspension, add weight fraction again and be the catalyzer of 0.1-0.3% (with respect to the weight of ceramic powder) and slowly be warmed up to 60-80 ℃ and keep constant temperature more than 30 minutes, promptly obtain the solidified base substrate, then with the base substrate demoulding, drying, and sintering obtains porous ceramics.Above-mentioned several patent of invention all need add a large amount of one-tenth (making) hole agent in composite base-material, form porous ceramics by becoming (making) hole agent gasification when the high temperature sintering.Chinese invention patent " a kind of employing high molecular polymerization crosslinking solidified porous ceramics extrinsion pressing " (application number 98109145) adopts high molecular polymerization crosslinking solidified porous ceramics extrinsion pressing, based on existing extrinsion pressing, when making, wet base adds by acrylamide (AM) and N, organic monomer and initiator thereof that N '-methylene-bisacrylamide (MBAM) forms, the extrusion molding post-heating makes the organic monomer polymerization crosslinking in the wet base substrate, and is dry and burn till.This method needs after the green compact heating organic monomer polymerization crosslinking in the base substrate to be solidified.
In sum, there is the deficiency of two aspects in porous ceramics at present, and the one, add (making) hole agent, the precision of porous ceramics is affected, the 2nd, need after the green compact heating organic monomer polymerization crosslinking in the base substrate to be solidified.
The preparation of porous metal material generally all is to adopt powder metallurgy forming method, casting, sedimentation etc., for the porous metal that are used for micro-filtration, adopts the powder metallurgy forming method more, as compression molding, isostatic pressing method, powqder rolling process and the moulding of powder slurry extrusion process.Chinese invention patent " manufacture method of porous metal (application number 00130308) is filled between the salt powder molten metal by pressurization; again the mixture heating up of pulverous salt and metal-powder to lower than the melt temperature of salt, than the high temperature of the melt temperature of metal-powder; make above-mentioned metal powders melt, from above-mentioned molding, porous metal finally made in the salt stripping again.In fact, this also is a kind of forming method that adds pore former.
In sum, though the preparation method of present existing inorganic porous material is many, there is following deficiency:
(1) mostly need to add the pore former of some amount, the gasification by pore former in high temperature sintering produces required hole, and the aperture is bigger, is prone to defective.
(2) green strength is poor after the moulding, though have good intensity can be arranged, need under the condition of heating reaction to solidify.
(3) it is long that base substrate solidifies time of drying.
(4) different materials need adopt different preparation methods with shape, for example preparation of porous metal and porous ceramics, and the preparation of pipe, sheet may will be adopted diverse ways.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of and need not add pore former, have preparation method than the porous inorganic microstraining core of Johnson ﹠ Johnson's base intensity, suitable multiple shape.
Another object of the present invention is to provide a kind of porous inorganic microstraining core that has than Johnson ﹠ Johnson's base intensity, suitable multiple shape.
Principle of the present invention is: need not add (making) hole agent, but obtain hole by bridge formation, the control sintering temperature of ceramics powder itself, obtain the micro-filtration porous ceramics of 0.1-10 μ m by the raw material of selecting the different-grain diameter scope for use.Just making behind the porous ceramic shaping at short notice can self-vulcanizing, obtains the good green compact of intensity, optimize porous ceramics production technique, shorten the production cycle, improve the green compact yield rate, obtain the micro-filtration porous ceramics of high weight.
Purpose of the present invention realizes as follows: comprise the steps:
(1) curing additive of the carrier of 100 parts by weight base-materials, 8-30 parts by weight and 2-20 parts by weight is mixed after, stirred 2-4 hour, make composite base-material;
(2) composite base-material is made type at mould inner pressure, and reaction is solidified, and makes the porous green compact;
(3) the green compact demoulding, oven dry at 700 ℃～1550 ℃ sintering temperatures, soaking time 1-2 hour, are made the inorganic porous filter core of micro-filtration after the cooling;
Described base-material comprises one or more the mixture in metal nickel powder, titanium valve or the Stainless Steel Powder, or one or more the mixture in the silica powder, aluminum oxide powder, diatomite in powder, trichroite powder; Described carrier comprises water or ethanol.Described curing additive comprises organism curing additive or inorganics curing additive.
Reactant in the curing additive in the composite base-material of the present invention is the organic and inorganic compound with specified property, and the curing that reacts under at room temperature can the solidifying agent effect in curing additive of these compounds makes green compact have good intensity.The organism curing additive is made up of reactant and solidifying agent,
The thing that responds in the composite base-material additive can be acrylate, Resins, epoxy, urethane, a resol room temperature generation crosslinking polymerization under the solidifying agent effect of correspondence, make the green compact of compression moulding have good green strength, the demoulding then, this green compact with good strength, can guarantee the integrity of green compact in the knockout course, in handling process, be not easy brokenly base, improved yield rate greatly, can effectively reduce cost.
Raolical polymerizable under the effect of isopropyl benzene hydroperoxide, just can take place in acrylate at ambient temperature, and monomer generation graft copolymerization, curing make base substrate have intensity.
Exist triatomic ring in the structure of Resins, epoxy, have very strong open loop ability and special Cloud Distribution, cause the epoxy reaction activity very high, under the effect of organic amine solidifying agent, react with the reactive hydrogen atom that contains in the amine, cross linking of epoxy resin is solidified.
Base polyurethane prepolymer for use as is cross-linked to form polymkeric substance under the effect of low molecular weight polyols or polyamine curing agent, base substrate is solidified.
The condensation reaction of methylol takes place in resol under acid as curing agent effects such as hydrochloric acid, mahogany acid, phosphoric acid, the resol crosslinking polymerization becomes tridimensional network, makes green compact have suitable intensity.
Additive in the composite base-material can be urea and corresponding lytic enzyme----urine enzyme, utilize the urine enzyme catalyst in efficient catalytic performance that room temperature had, urea is under the effect of urine enzyme catalyst, and the water in urea and the green compact reacts, and need not heat just to make green compact drying and dehydrating curing at room temperature.
Solidifying agent in the composite base-material also can be a mineral compound, by adding mineral compound, composite base-material is at room temperature solidified after moulding.Solidifying agent is that the additive of mineral compound is an inorganic coagulation material, can be the hydraulicity and air-setting according to the difference of curing condition.Body material after the inorganic coagulation material that adds the hydraulicity fully mixes, compression moulding, inorganic coagulation material and water generation hydration, the formation hydrate, thus make the green compact setting and harden, have good green strength.Hydraulic response type inorganic coagulation material of the present invention is silicate cement, aluminate cement and gypsum.
After silicate cement and base-material and the water mixing and stirring, the Dicalcium Phosphate (Feed Grade) of cement surface, tricalcium silicate, tricalcium aluminate and tetracalcium aluminoferrite etc. and water generation hydration form corresponding hydrate, separate out with colloidal particle, and condense gradually and become gel, through the certain hour post-hardening.
The essential mineral composition of aluminate cement is monocalcium aluminate, calcium dialuminate.Wherein monocalcium aluminate sclerosis is to be the main source of initial strength of the porous ceramic micro filter filter core of additive with the aluminate cement rapidly.
The main component of gypsum is a hydrous calcium sulfate.After porous ceramic micro filter filter base-material and gypsum and water mixing and stirring and the compression moulding, semi-hydrated gypsum wherein and water reaction, again aquation generates dihydrate gypsum and emits heat and setting and harden gradually, the hydrate crystal continues to form in a large number, grow up later on, be in contact with one another between the crystal and adhesion, form the crystallization network forming, make the base substrate sclerosis.
Remove hydraulicity inorganic coagulation material, the porous inorganic microstraining core of self-vulcanizing can also adopt the inorganic coagulation material of air-setting.Gas-solid reaction type inorganic coagulation material of the present invention is phosphoric acid salt, calcium hydroxide, alkalimetal silicate, water glass and silicon sol etc.After compression moulding, place required atmosphere (air or CO
2Gas) in, active ingredient in the green compact and corresponding gas reaction are solidified base substrate and are had good intensity.
These can react in room temperature, form crosslinked, the additive that solidifies or dewater is not subjected to the influence of porous inorganic microstraining core base-material, no matter be nickel, titanium, stainless steel, bronze, the metal substrates of metal powder classes such as copper, or silicon oxide, aluminum oxide, diatomite, perlite, quartz sand, the ceramic base-material of ceramics powder classes such as trichroite, or wherein a kind of or the mixed powder of two kinds of compositions wherein, can be to wherein adding by organic, mineral compound and corresponding catalyzer and/or solidifying agent thereof, these compounds at room temperature can be in additive catalyzer or the solidifying agent effect under solidify, make green compact have good intensity.Adopt this self-vulcanizing forming method, can be pressed into tubulose, disk shape, bowl-shape, hemispherical and bullet-shaped.Green strength is good, can effectively improve the yield rate of base substrate.After the demoulding, dry and sintering can obtain the porous inorganic microstraining core of the few different shape of defective.
The present invention compared with prior art has following advantage:
(1) need not add pore former.
(2) base substrate at room temperature reacts curing, has good green strength.
(3) be applicable to difform filter core preparations such as tubulose, disk shape, bowl-shape, hemispherical and bullet-shaped.
Not only be applicable to the preparation of porous ceramic filter element but also can be used for preparing porous metal.
Be described in further detail the present invention below by embodiment.
Embodiment
Below the specific embodiment of the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Earlier urea, the 0.5 weight part urine enzyme with 2.5 weight parts is dissolved in the carrier water of 20 weight parts, is that the aluminum oxide powder base-material of 10 μ m mixes with 100 weight part median sizes again, is mixed with composite base-material, through 2 hours mechanical stirring, makes uniform composite base-material.Composite base-material is added in the round mould of hollow, and compacting was placed 1 hour, under the effect of urine enzyme, urea in the base substrate and water generation hydrolysis reaction, make the moisture removal in the base substrate, reach the exsiccant purpose, base substrate solidifies, obtain intensity, the demoulding, green compact are through further dry, sintering, and sintering temperature is 1550 ℃, soaking time 1 hour promptly obtains the porous alumina sheet after the cooling.
After testing, gained porous alumina sheet microstraining core mean pore size is about 2 μ m, and porosity is about 38%, and diameter 100mm, thickness are 5mm.This porous alumina sheet intensity is good, except that can be used for water, air and other fluidic micro-filtration, also can be used as porous support, modifies and modification functional membranes such as preparation nanometer film.
Embodiment 2
Earlier the gypsum with 20 weight parts is dissolved in the carrier water of 30 weight parts, is that the diatomite in powder base-material of 10 μ m mixes with 100 weight part median sizes again, is mixed with composite base-material, through 3 hours mechanical stirring, makes uniform composite base-material.Composite base-material is added after the cast mould inner pressure makes type, semi-hydrated gypsum wherein and water reaction, again aquation generates dihydrate gypsum and emits heat and setting and harden gradually, the hydrate crystal continues to form in a large number, grow up later on, be in contact with one another between the crystal and adhesion, form the crystallization network forming, make the base substrate sclerosis.The demoulding then, green compact are through further dry, sintering, and sintering temperature is 1110 ℃, and soaking time 2 hours promptly obtains tubular porous diatomite filter core after the cooling.After testing, mean pore size is about 0.3 μ m, and porosity is about 55%, and diameter 120mm, thickness are 8mm, high 100mm.
Diatomite is a kind of biogenic silicastone, mainly by ancient times diatom and other microorganism siliceous remains form, main component is opal and mutation thereof, diatom in the diatomite has many different shapeies, as discoid, needle-like, tubular, pinniform etc., the high 80-90% of reaching of aperture, porosity that countless gaps are arranged on the silicon shell, diatomaceous operational characteristic is characteristics such as fine and smooth, loose, light weight, porous, suction and perviousness be strong.The tubular porous diatomite filter core that present embodiment is made has very high porosity and has big flux.Can be used for fluidic such as water and air and filter, objectionable impuritiess such as the dust in can the filtering fluid, suspended contaminant, microorganism.
Embodiment 3
Earlier the calcium hydroxide with 10 weight parts is dissolved in the carrier water of 15 weight parts, is that the silicon dioxide powder base-material of 10 μ m mixes with 100 weight part median sizes again, is mixed with composite base-material, through 3 hours mechanical stirring, makes uniform composite base-material.Composite base-material is added in the bullet-shaped mould, and extrusion molding feeds CO
2Base substrate is solidified, obtain desirable strength, the demoulding, drying, at 1300 ℃ of sintering, soaking time 1 hour promptly obtains bullet-shaped porous silica filter core after the cooling.
After testing, gained porous silica filter core mean pore size is about 10 μ m, and porosity is about 40%, and diameter 38mm, thickness are 8mm, high 75mm.The pre-filtering filter core that can be used as micro-filtration removes suspended substance, dust and pollutents such as algae, red worm in anhydrating.
Embodiment 4
Isopropyl benzene hydroperoxide with 1.8 parts by weight of acrylic esters, 0.2 weight part is dissolved in the carrier ethanol of 20 weight parts earlier, be that 10 μ m metallic titanium powder base-materials mix with the median size of 100 weight parts again, be mixed with composite base-material,, make uniform composite base-material through 3 hours mechanical stirring.Composite base-material is added in the disk pattern tool, and compacting was placed 1 hour, under the effect of isopropyl benzene hydroperoxide, and the acrylate generation Raolical polymerizable in the base substrate, monomer generation graft copolymerization, curing make base substrate have intensity.The demoulding, green compact are through oven dry, inert atmosphere sintering, and sintering temperature is 1100 ℃, and soaking time 1 hour promptly obtains porous metal titanium sheet after the cooling.
After testing, gained porous metal titanium sheet filter core can obtain the porous metal titanium sheet that mean pore size is about 2 μ m, and porosity is about 40%, and diameter 150mm, thickness are 3mm.This porous metal titanium sheet intensity is good, can be used for water, air and other fluidic micro-filtration, removes the suspended substance in the fluid, also can be used for aeration.
Embodiment 5
Resol, 0.4 mahogany acid catalyzer with 2.6 weight parts is dissolved in the carrier ethanol of 20 weight parts earlier, be that 20 μ m, 316 Stainless Steel Powder base-materials mix with the particle diameter of 100 weight parts again, be mixed with composite base-material,, make uniform composite base-material through 3 hours mechanical stirring.Composite base-material is added in the bullet-shaped mould, compacting, resol carries out polymerizing curable under the mahogany acid catalyst action, make base substrate have intensity, the demoulding, green compact are through further dry, the hydrogen reduction atmosphere sintering, sintering temperature is 1050 ℃, and soaking time 1 hour promptly obtains bullet-shaped Porous Stainless Steel filter core after the cooling.After testing, mean pore size is about 5 μ m, and porosity is about 45%, and diameter 38mm, thickness are 3mm, high 100mm.The micro-filtration that can be used as water removes suspended substance, dust and pollutents such as algae, red worm in anhydrating, also can be used as the purification of air, removes airborne dust, microorganism etc.
Embodiment 6
Water glass with 3 weight parts is dissolved in the carrier water of 8 weight parts earlier, is that 3 μ m metal nickel powder base-materials mix with the particle diameter of 100 weight parts again, is mixed with composite base-material, through 3 hours mechanical stirring, makes uniform composite base-material.Composite base-material is added in the mould of cast, extrusion molding, and feed CO
2Base substrate is solidified.The demoulding, drying, 700 ℃ of vacuum sinterings, soaking time 1 hour promptly obtains cast porous-metal nickel filter core after the cooling.After testing, mean pore size is about 0.5 μ m, and porosity is about 41%, and diameter 45mm, thickness are 3mm, high 200mm.Can be used as purification, degerming and the clarification of other fluidic, the micro-filtration of water and air, also can be used as porous support.
Embodiment 7
Water glass with 10 weight parts is dissolved in the carrier water of 20 weight parts earlier, be that the trichroite powder base-material of 8 μ m mixes with 100 weight part particle diameters again, be mixed with composite base-material, through 2 hours mechanical stirring, after stirring, composite base-material is added in the sheet semisphere mould compression moulding, the base substrate sclerosis back demoulding, green compact are through further dry, sintering, sintering temperature is 1250 ℃, and soaking time 1 hour promptly obtains semisphere porous cordierite filter core after the cooling.After testing, mean pore size is about 0.1 μ m, and porosity is about 48%, and diameter 120mm, thickness are 6mm, high 60mm.
Embodiment 8
Earlier the silicate cement with 10 weight parts is dissolved in the carrier water of 30 weight parts, is that the perlite powder base-material of 10 μ m mixes with 100 weight part particle diameters again, is mixed with composite base-material, through 4 hours mechanical stirring, makes uniform composite base-material.Composite base-material is added in the round mould, and compacting is in blocks, the Dicalcium Phosphate (Feed Grade) on silicate cement surface, tricalcium silicate, tricalcium aluminate and tetracalcium aluminoferrite etc. and water generation hydration, form corresponding hydrate, separate out with colloidal particle, and condense gradually and become gel, through the certain hour post-hardening, make base substrate have intensity, the demoulding, green compact are through further dry, sintering, and sintering temperature is 1110 ℃, soaking time 1 hour promptly obtains flake porous perlite filter core after the cooling.After testing, mean pore size is about 0.4 μ m, and porosity is about 65%, and diameter 150mm, thickness are 15mm.
Claims (8)
1, a kind of preparation method of porous inorganic microstraining core is characterized in that comprising the steps:
(1) curing additive of the carrier of 100 parts by weight base-materials, 8-30 parts by weight and 2-20 parts by weight is mixed after, stirred 2-4 hour, make composite base-material;
(2) composite base-material of (1) preparation is made type at mould inner pressure, reaction is solidified, and makes the porous green compact;
(3) with the green compact demoulding, the oven dry of (2) preparation,, soaking time 1-2 hour, make the inorganic porous filter core of micro-filtration after the cooling at 700 ℃～1550 ℃ sintering temperatures;
Described base-material comprises one or more the mixture in metal nickel powder, titanium valve or the Stainless Steel Powder, or one or more the mixture in the silica powder, aluminum oxide powder, diatomite in powder, trichroite powder; Described carrier comprises water or ethanol; Described curing additive comprises organism curing additive or inorganics curing additive.
2, according to the preparation method of the described porous inorganic microstraining core of claim 1, it is characterized in that: described organism curing additive comprises reactant and solidifying agent.
3, according to the preparation method of the described porous inorganic microstraining core of claim 2, it is characterized in that: described reactant is an acrylate, and solidifying agent is an isopropyl benzene hydroperoxide; Or reactant is resol, solidifying agent hydrochloric acid or mahogany acid or phosphoric acid; Or reactant is urea, and curing catalysts is the urine enzyme.
4, according to the preparation method of the described porous inorganic microstraining core of claim 1, it is characterized in that: described inorganics curing additive is solidified hydraulicity inorganic coagulation material or an air-setting inorganic coagulation material under the room temperature.
5, according to the preparation method of the described porous inorganic microstraining core of claim 4, it is characterized in that: the inorganic coagulation material of the described hydraulicity comprises silicate cement, aluminate cement or gypsum; The inorganic coagulation material of described air-setting is phosphoric acid salt, calcium hydroxide, alkalimetal silicate or water glass.
6, the prepared porous inorganic microstraining core of the described porous inorganic microstraining core preparation method of claim 1.
7, according to the described porous inorganic microstraining core of claim 6, it is characterized in that: described porous inorganic microstraining core be shaped as tubulose, disk shape, bowl-shape, hemispherical or bullet-shaped.
8, according to claim 6 or 7 described porous inorganic microstraining cores, it is characterized in that: described porous inorganic microstraining core mean pore size is 0.1um～10um; Porosity is 38%～65%; Thickness is 3～15mm.
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