CN104311095B - The method that porous ceramics is prepared with activated alumina presoma - Google Patents
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Abstract
Activated alumina presoma is prepared using inorganic aluminate the present invention relates to one kind, ceramic fibre and ceramic powder is added, filtration washing, is molded, burns till, high intensity, the method for high porosity ceramic is made.Bonus point powder and short ceramic fibre into inorganic aluminum salting liquid, are added on generation precipitation in precipitant solution after being uniformly dispersed, then add ceramic powder, and presoma is made in filtration washing；Presoma is well mixed with bonding agent, be molded, dry after form high intensity green compact, the machining such as turning can be carried out as needed, then atmosphere sintering in two steps：Activated alumina in porcelain base is changed into alpha-aluminium oxide by the first step under reducing atmosphere or inert atmosphere, while organic matter is changed into carbon, second step volatilizees oxidation of coal under oxidizing atmosphere, so that porous ceramics is made.Foamed ceramics prepared by the inventive method, the foamed ceramics intensity more close than cost prepared by original technology is high, porosity is high.
Description
Technical field
The present invention relates to field of ceramic preparation technology.Specifically, it is related to one kind and active oxidation is prepared by inorganic aluminate
Aluminium presoma, add ceramic fibre and ceramic powder, filtration washing, be molded, burn till, high intensity, high porosity ceramic is made
Method.
Background technology
Porous ceramics has the spies such as chemical stability is high, low thermal conductivity and high temperature resistant, corrosion-resistant, intensity are high, rigidity is big
Point, is widely applied in fields such as metallurgy, chemical industry, environmental protection, the energy, biologies, such as fluid purification filtering, purification separation, urge
In terms of agent carrier, sound absorption damping, insulation material, biological and medicinal implant material, materials for wall and sensor material [Wang Hui,
Zeng Lingke, Zhang Haiwen, wait porous ceramics-green functional material Chinese potteries, 2002,38 (3);6-8].Especially as resistance to
The porous ceramics of high-temp and high-strength insulation material requires that the porosity is high, is preferably not less than 80vol%；Current its preparation method
Mainly there are following a few classes：
（1）Foaming rubber plastic material infusion process, proposed that its technical process was substantially such as by Schwartzwalder in 1963
Under:It is first that the rubber and plastic object of foam form is shaped, then impregnated with ceramic slurry, extrude unnecessary slurry simultaneously
Dry, finally burn out rubber and plastic object, sinter the ceramic layer of residual.The shortcoming of this method is to release big when polymer template is discharged
Toxic gas is measured, environmental pollution is caused.
（2）By solvent of water by gel casting forming after, porous body, such as the U.S. are generated using freeze-drying mode
Patent USP8262957 (2012) and Application No. 201110247169.3 application documents, the shortcoming of this method is drying equipment
Investment is big, energy consumption is too high, low production efficiency.
（3）Casting generation porous body, such as Application No. after slurry are prepared with water, polymer and ceramic powder
200610124005.0 Chinese patent application is that alumina powder and water are mixed with into ceramic slurry, is added according to alumina powder
The converted starch of 30-5Ovol% ratio, it is uniform through ball milling mixing, ceramic slurry is injected in mould after degassing, 60- is heated to
85 DEG C are incubated 5-60 minutes, are stripped the sintered rear acquisition product of dried base substrate.In Application No. 201210148603.7
State's patent proposition flour turns into porous green compact with ceramic powder mixed fermentation, re-sinters the method as porous ceramics, and it is led
Have the disadvantage that consumption polymer is too many（Such as flour volume is more than ceramic powder volume）, green strength it is low.
（4）With injection molding after nitrogen gas foaming, porous body, such as Application No. are synthesized by radical polymerization
200810016714.6 patent application, takes monomer, the foaming agents such as ceramic powder and water, acrylamide to be made into slurry, in nitrogen
Strong stirring certain time in environment, as foam state, then additional initiator and catalyst continue to stir 0.5-3 minutes
To porous slurry, porous slurry is injected in unwetted mould, room temperature is placed -48 hours 1 minute under nitrogen protection, Ran Hou
The time is -6 hours 10 minutes curing moldings at a temperature of 150 DEG C of 60-, is then stripped drying, is less than the moisture content of base substrate
0.5 below wt%, then burns till under certain condition.The major defect of this method be the cost operated in nitrogen it is very high and
And dried blank strength is very low.Although also have using acrylamide monomers with slurry, foamed with air, gel injection-moulding into
Type, but because oxygen has inhibition to radical polymerization, the blank strength for causing this method to prepare is lower.
It is made into organic solvent plus ceramic powder after slurry, gel casting forming and removes organic solvent generation porous body,
Adding by solvent of the tert-butyl alcohol for the proposition such as Chen R F removes tertiary fourth after organic monomer and ceramic powder, gel casting forming
Alcohol generates porous body（Ceramics with ultra-low density fabricated by gelcasting:An
Unconventional view, Journal of the American Ceramic Society. Chen R F, Huang
Y, Wang C A,et al. J. Am. Ceram. Soc., 2007,90(11): 3424-3429.）；Application No.
200910071845.9 patent document proposition acetamide etc. be solvent.The major defect of this kind of method is organic solvent to ring
Border harm is serious and cost is very high.
The content of the invention
Activated alumina typically refers to gama-alumina or η-aluminum oxide, and they have the spinelle for including more defect
Structure, and due to excellent surface nature, larger, the strong surface adsorption property of such as surface area, surface acidity center, with
And loose structure, it is widely used as catalyst, carrier, adsorbent is dried, applied to petrochemical industry, Organic Chemical Industry, chemical fertilizer work
Industry and environmental protection industry.Activated alumina is actually the agglomerate coalesced by crystallite particles, is existed in the inside of agglomerate
The micropore differed in size.
In order to overcome existing high intensity, high porosity porous ceramics processing cost height, etc. serious to environmental hazard no
Foot, the present invention proposes following solution：Technology of preparing of the reference catalyst carrier field on activated alumina, to inorganic aluminum
Add short ceramic fibre and organic dispersing agent in salting liquid, the generation precipitation such as precipitating reagent is added after being uniformly dispersed；Again plus ceramic powder simultaneously
Stir evenly, filtration washing；Filter cake is well mixed with organic bond, be molded, dry after formed high intensity green compact；As needed may be used
The machining such as turning is carried out, then the atmosphere sintering in two steps in high temperature furnace.The first step is under reducing atmosphere or inert atmosphere
Activated alumina in porcelain base is changed into Alpha-alumina, and organic matter is changed into carbon simultaneously；Second step waves oxidation of coal under oxidizing atmosphere
Hair, so that porous ceramics is made.
The preparation of activated alumina, is usually to form the presoma specially prepared in 400-700 DEG C of roasting.Prepare forerunner
The method of body can be divided into three classes by primary raw material used：（1）The inorganic aluminate precipitation method, the precursor species form prepared by this method
Belonging to the boehmite with open structure, [Liu's winter, Ye Zhiliang, Cao Jing wait the aluminium salt precipitation method to prepare low heap softer than a false water
The research Progress ＆ New Products of aluminium stone, 2003,17 (7):29-32.] or the aluminium carbonate ammonium [such as Yang Yong, Ning Guiling, Lin Yuan
The development investigation of materials journals of aluminium carbonate ammonium, 1999,13 (3):269-274]；（2）Aluminium alcoholates Hydrolyze method；（3）Aluminium hydroxide is fast
Fast evaporation.The inorganic aluminate precipitation method are lower than aluminium alcoholates Hydrolyze method cost, than aluminium hydroxide rapid dehydration method simple equipments, are current
Using more method.The present invention is exactly to prepare activated alumina presoma using the inorganic aluminate precipitation method, then with ceramic powder
Etc. preparing porous ceramics.
Activated alumina is changed into Alpha-alumina at 800-1500 DEG C, and multiple crystallite particles coalescences are combined into Alpha-alumina
More than crystal, particle size increase decades of times, inside particles hole and the interparticle hole overwhelming majority disappear, generally can not structure
Into the porous ceramics of high porosity.This has had no many with activated alumina preparation since being probably porous ceramic technology development many decades
The reason for hole is ceramic.
In order that activated alumina inside particles hole and the interparticle hole overwhelming majority are remained in the porcelain body of sintering,
The present invention does not directly prepare porcelain with activated alumina and prepares porous ceramics, but prepares porcelain system with activated alumina presoma
Standby porous ceramics.Organic dispersing agent and organic bond are added when preparing activated alumina presoma, and uses two step gas
Atmosphere sintering process.The control climate technology that the first step is sintered with reference to non-oxidized substance fine ceramics, in reducing atmosphere or inert atmosphere
Under, make organic bond is heated to be changed into carbon particulate, at the same time presoma is heated is converted into activated alumina；Countless carbon particulates
It is interspersed between activated alumina particulate, hinders the mutual coalescence of activated alumina particle phase to combine.It is living as temperature is further raised
Property aluminium oxide particles are progressively changed into alpha-alumina particle, and the inside and outside of these alpha-alumina particles all has carbon particulate.Second step
By carbon particulate voloxidation under oxidizing atmosphere, because no longer occurring the Phase change shrinkage of aluminum oxide during this, shared by carbon particulate
Space is remained in the porcelain body of sintering as hole, so that porous ceramics is made.The present invention is chemical field on active oxidation
The control climate technology of the standby a part of technology of aluminum and non-oxidized substance fine ceramics sintering, skill is prepared with oxide special cermacis
Art is organically combined, and it is innovative that this cross-cutting technology, which is combined, is not apparent.
Embodiment
In order to prepare high intensity, porous ceramics, the present invention changes to the existing method for preparing activated alumina presoma
Enter, organic dispersing agent and short ceramic fibre are added into the solution being made into inorganic aluminate and water, precipitating reagent is added on after being uniformly dispersed
In solution, generation precipitation；Again plus ceramic powder, stir evenly, filtration washing；Filter cake is well mixed with organic bond, is molded, does
High intensity green compact are formed after dry, the machining such as turning can be carried out as needed, then the atmosphere sintering in two steps in high temperature furnace.
The first step rises to 300 DEG C or so with 2-9 DEG C/min programming rate under reducing atmosphere or inert atmosphere, then with 0.3-3 DEG C/
Min programming rate rises to 800 DEG C or so from 300 DEG C or so（Organic dispersing agent and organic bond, which are heated, during this is changed into carbon
Particulate, at the same time presoma is heated is converted into activated alumina）, then with 1-7 DEG C/min programming rate from 800 DEG C or so
Rise to sintering temperature（Active oxidation aluminum particulate is progressively changed into alpha-alumina particle during this）；Second step uses oxidizing atmosphere instead,
1-6h is incubated at a sintering temperature, oxidation of coal is volatilized, so that porous ceramics is made；The preferred range of sintering temperature is in 1200-
Between 1600 DEG C.
Described inorganic aluminate, including acid mineral aluminium salt and the class of basic mineral aluminium salt two.Acid mineral aluminium salt includes nitre
Sour aluminium, aluminium chloride, aluminum sulfate, alum, its precipitating reagent include ammoniacal liquor, sodium hydroxide, ammonium carbonate, ammonium hydrogen carbonate, meta-aluminic acid
Sodium；Basic mineral aluminium salt includes sodium metaaluminate and potassium metaaluminate, and its precipitating reagent includes hydrochloric acid, sulfuric acid, nitric acid, acetic acid, formic acid, with
And acid mineral aluminium salt.Acid mineral aluminum salt solution preferred concentration is 0.1-1.5mol/L, and basic mineral aluminum salt solution is preferably dense
Spend for 0.4-5.0mol/L, the pH value that the ratio of inorganic aluminate and precipitating reagent completes Mother liquor by precipitation is advisable between 7-10.
Described organic dispersing agent includes：The water soluble starch derivatives such as pre-gelatinized starch, maltodextrin, hydroxy ethyl fiber
The water-soluble cellulose derivatives such as element, polyethylene glycol, oxygen ethylene copolymer, polyacrylate, citrate.Often add 100g without
Machine aluminium salt correspondence adds 0.1-9.0g organic dispersing agents.
Described ceramic powder includes：High temperature alumina, flint clay, kaolinite, quartz, feldspar, talcum, wollastonite, olive
Olive stone, spinelle, zirconium oxide, yittrium oxide, calcium carbonate, magnesia, dolomite；Particle diameter is 10nm-30 μm, often adds 100g
Inorganic aluminate correspondence adds 10-100g ceramic powders.
Described organic bond includes：Starch, modified starch, hydroxyethyl cellulose, guar gum, modified guar, field
Cyanines glue, modified sesbania gum, polyacrylamide, polyvinyl alcohol, alginate, polyacrylate.Often add 100g inorganic aluminates pair
7.0-75g organic bonds should be added.
Embodiments of the present invention are illustrated below:
Embodiment 1
First workshop section：It is prepared by presoma.Take the water aluminum nitrates of 375g nine to be dissolved in 1.5kg water, plus 7.5kg maltodextrins as point
After powder, stirring and dissolving, plus 90g alumina fibres（Length 2-7mm）, stir 2h and disperse to fiber substantially uniformity, obtain aluminum nitrate
Solution；Take 320g sodium metaaluminates to be dissolved in 1.2kg water, obtain precipitant solution.At room temperature, the aluminum nitrate solution prepared slowly
It is added in the precipitant solution that fiercely stirred, is subsequently added 200g high temperature aluminas（It is ground to 1.3 μm of median in advance）、
20g light magnesium oxides, continue that 1h is stirred at room temperature；Suction filtration, in semi-solid, add 70ml water, drained to filter cake on filter cake；So
Repeated washing filter cake 3 times.
Second workshop section：With porcelain, shaping, drying, burn till.Washed filter cake is transferred in batch mixer, plus 60g pre-gelatinized
Starch, is transferred in vinyl disc after being well mixed at room temperature, makes thinner, dry in the air 4h at room temperature；Compressing is 10mmX10mmX60mm
Four stupefied cylinders, 60 DEG C drying, obtain high intensity green compact；Co-pressed 60 green compact, the green compact for taking a part to dry are put into controllable
In the high-temperature electric resistance furnace of atmosphere, 290 DEG C are risen in a nitrogen atmosphere with 5 DEG C/min；Hereafter, 800 DEG C are risen to 1 DEG C/min, followed by
With 3 DEG C/min 1550 DEG C are risen to from 800 DEG C；Last constant temperature 3h in air atmosphere.200 DEG C are naturally cooling to stove.
Thus the average bending strength of porous ceramics prepared is 1.65MPa, and mean porosities are 86vol%.
Comparative example 1
Take 15 from the green compact that embodiment 1 is suppressed and is dried, be put into the high-temperature electric resistance furnace of controlled atmosphere, using with reality
The identical of example 1 heating temperature control program is applied, simply air atmosphere is taken always therebetween, prepared porous ceramics hole rate is
39vol%, it can be seen that, do not use two step atmosphere sintering methods to reach the target of high porosity.
Embodiment 2
First workshop section：It is prepared by presoma.Take 6.6kg hydrazine aluminum sulfates to be dissolved in 10kg water, plus 0.1kg ammonium citrates, stir
After dissolving, plus 1.2kg alumina fibres（Length 2-7mm）, stir 3h and disperse to fiber substantially uniformity, obtain aluminum sulfate solution；Take
5.7kg ammonium carbonates are dissolved in 9kg water, obtain precipitant solution；At room temperature, the aluminum sulfate solution prepared slowly is added on and fiercely stirred
In the precipitant solution mixed, it is subsequently added the composite ceramic powder being made up of 1.6kg flint clays, 0.4kg quartz and 0.2kg feldspars
（It is pre-mixed and is ground to 1.8 μm of median）, continue that 1h is stirred at room temperature；Suction filtration, in semi-solid, adds to filter cake on filter cake
160ml water, is drained；Such repeated washing filter cake 3 times；Washed filter cake is transferred in stainless steel disc, 70 DEG C of drying obtain powdery
Presoma.In mass production, can by Chemical Manufacture enterprise carry out presoma preparation, for Production of Ceramics enterprise with porcelain, into
Type, drying, burn till.
Second workshop section：With porcelain, shaping, drying, burn till.By the powdery precursor prepared from the first workshop section and 280g starch
Mixing, plus 3.5kg water, the stainless steel mould that injection cavity size is 200mmX200mmX70mm after being well mixed at room temperature
It is interior, 2h is incubated in 90 DEG C of baking ovens, the wet base substrate as gelling properties；The demoulding, 60 DEG C of drying, obtains high intensity green compact；A part
The four stupefied cylinders that size is 10mmX10mmX60mm are cut into, are put into using natural gas as the shuttle kiln of fuel, air mistake is controlled
Surplus coefficient is 0.93（Reducing atmosphere）, 300 DEG C are risen to 1h time, followed by slow heating rises to 800 with 7h time
DEG C, hereafter rise to 1370 DEG C from 800 DEG C with 3h time；It is 1.12 finally to control coefficient of excess air（Oxidizing atmosphere）,
1370 DEG C of insulation 2h.200 DEG C are naturally cooling to stove.
Thus the average bending strength of porous ceramics prepared is 1.29MPa, and mean porosities are 81vol%.
Comparative example 2
Four stupefied small 20, the green compact of cylinder that size is 10mmX10mmX60mm are cut from the big green compact obtained by embodiment 2,
It is put into using natural gas as the shuttle kiln of fuel, using heating temperature control program same as Example 2, simply controls always therebetween
Coefficient of excess air is 1.12（Oxidizing atmosphere）, prepared porous ceramics mean porosities are 32vol%, it can be seen that, no
The target of high porosity cannot be reached using two step atmosphere sintering methods.
From above-described embodiment as can be seen that foamed ceramics prepared by the inventive method, the cost prepared than original technology
Close foamed ceramics intensity is high, porosity is high.These embodiments are used for the explanation to claim, but are not intended to right
It is required that restriction, protection scope of the present invention should be defined by claims.
Claims (1)
1. a kind of method that porous ceramics is prepared with activated alumina presoma, it is characterised in that：Including Liang Ge workshop sections, the first work
Section prepares presoma, organic dispersing agent and short ceramic fibre is added into the solution being made into inorganic aluminate and water, after being uniformly dispersed
Generation precipitation in precipitant solution is added on, then adds ceramic powder and stirs evenly, filtration washing obtains presoma；Second workshop section with porcelain,
Shaping, dry, sintering, presoma is well mixed with organic bond, be molded, dry after formation high intensity green compact, Ran Hou
Atmosphere sintering in two steps in high temperature furnace, first step reducing atmosphere or inert atmosphere, first with 2-9 DEG C/min programming rate liter
From 300 DEG C 800 DEG C are risen to 300 DEG C, then with 0.3-3 DEG C/min programming rate, then with 1-7 DEG C/min programming rate
Sintering temperature is risen to from 800 DEG C；Second step uses oxidizing atmosphere instead, and 1-6h is incubated at a sintering temperature；Sintering temperature is in 1200-
Between 1600 DEG C；Described inorganic aluminate, including acid mineral aluminium salt and the class of basic mineral aluminium salt two, acid mineral aluminium salt include
Aluminum nitrate, aluminium chloride, aluminum sulfate, alum, its precipitating reagent include ammoniacal liquor, sodium hydroxide, ammonium carbonate, sodium carbonate, bicarbonate
Sodium, ammonium hydrogen carbonate, sodium metaaluminate；Basic mineral aluminium salt includes sodium metaaluminate and potassium metaaluminate, and its precipitating reagent includes hydrochloric acid, sulphur
Acid, nitric acid, acetic acid, formic acid, and acid mineral aluminium salt；Acid mineral aluminum salt solution concentration is 0.1-1.5 mol/L, alkaline nothing
Machine aluminum salt solution concentration is 0.4-5.0 mo1/L, and the ratio of inorganic aluminate and precipitating reagent is according to the pH value of precipitation reaction Mother liquor
Determined between 7-10；Described ceramic powder includes：High temperature alumina, flint clay, kaolinite, quartz, feldspar, talcum, silicon
Lime stone, olivine, spinelle, zirconium oxide, yittrium oxide, calcium carbonate, magnesia, dolomite, particle diameter are that l0 nanometers -30 are micro-
Rice, often adds 100g inorganic aluminates correspondence and adds 10g-100g ceramic powders.
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| CN111410542B (en) * | 2020-03-18 | 2021-04-16 | 中国科学院上海硅酸盐研究所 | Porous ceramic with uniformly distributed sub-micropores prepared by using inorganic eutectic salt and preparation method thereof |
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| CN113427002B (en) * | 2021-06-25 | 2022-06-21 | 哈尔滨工业大学 | Pressureless sintering preparation method of three-dimensional porous structure |
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| CN101591164A (en) * | 2008-05-30 | 2009-12-02 | 山东理工大学 | The preparation method of alumina porous ceramic |
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| CN101139206A (en) * | 2007-08-13 | 2008-03-12 | 南京九思高科技有限公司 | Method for preparing low-temperature burnt porous ceramics support |
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