CN105645989B - The preparation method of meso-porous alumina ceramics - Google Patents
The preparation method of meso-porous alumina ceramics Download PDFInfo
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- CN105645989B CN105645989B CN201610143037.9A CN201610143037A CN105645989B CN 105645989 B CN105645989 B CN 105645989B CN 201610143037 A CN201610143037 A CN 201610143037A CN 105645989 B CN105645989 B CN 105645989B
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- dihydrogen phosphate
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- aluminium dihydrogen
- porous alumina
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- 239000000919 ceramic Substances 0.000 title claims abstract description 102
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 71
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910001593 boehmite Inorganic materials 0.000 claims abstract description 14
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims description 43
- 229910001648 diaspore Inorganic materials 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 238000009736 wetting Methods 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 21
- 239000002994 raw material Substances 0.000 abstract description 13
- 239000011230 binding agent Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009766 low-temperature sintering Methods 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000007493 shaping process Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 21
- 238000005452 bending Methods 0.000 description 14
- 239000007788 liquid Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000010791 quenching Methods 0.000 description 5
- 230000000171 quenching effect Effects 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000002370 organoaluminium group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A kind of preparation method of high specific surface area and mesoporous aluminium oxide ceramics, using aluminium dihydrogen phosphate as binding agent, meso-porous alumina ceramics are prepared using powder sintering.This method is mainly raw material with nanometer boehmite, and aluminium dihydrogen phosphate is binding agent, and powder is molded with pressed disc method and sinters synthesising mesoporous aluminium oxide ceramics at low temperature.The meso-porous alumina ceramics that the present invention synthesizes are the accumulation construction ducts using nano-particle; can be according to actually preparing required shape by powder shaping with pressed disc method; low-temperature sintering at the same time; the energy is saved; simplify preparation process; so that the production cycle shortens half, and it can realize the efficient production of scale.
Description
Technical field
The present invention relates to a kind of method for preparing meso-porous alumina ceramics, and in particular to one kind is former with nanometer boehmite
Material, aluminium dihydrogen phosphate aqueous solution (Al (H2PO4)3Aq binding agent) is made, it is controllable to prepare specific surface area using powder sintered method
Meso-porous alumina ceramics.
Background technology
Mesoporous material has larger specific surface area and pore volume, and controllable pore-size distribution, is adsorbing, and filters, catalysis
Have a wide range of applications Deng field, and meso-porous alumina (MA) is by the higher γ-Al of activity2O3Composition, specific surface area is big, inhales
Attached property is good, and stability is good, is commonly used for adsorbent, catalyst and catalyst carrier.Document 1 " Irandoust S, Anderson
B.A review of the selective reduction of NOX with hydrocarbons under lean
burn conditions with non-zeolitic oxide and platinum group metal catalysts
[J].Catalysis Review,1998,30(3):343-348. " propose γ-Al2O3Price is less expensive, it is relatively simple to prepare and can
With selective absorbing ion, not with reaction solid/liquid/gas reactions, do catalyst carrier when can improve the anti-Poisoning of catalyst, therefore in work
Industry and research field cause great concern.
Mesoporous block materials can solve powder body material be difficult to separation and caused by pollution problem, while but also with mesoporous powder
The various advantages of body material, its excellent performance make market stronger to its demand.Meso-porous alumina ceramics not only compare table
Area is big, has good pore volume while also intensity is high, wear-resistant, high temperature resistant, the good characteristic such as anticorrosive, can be severe
Used in the environment at quarter.It is sol-gal process to prepare the common method of mesoporous material at present.Document 2 " Liu Wei deep pools high porosities,
The preparation of high intensity, porous aluminium oxide ceramics and characterization [D] Tsinghua University, 2009. " proposition sol-gal processes can pass through tune
The pH value of section solution comes adjustment aperture size and specific surface area, is readily available micropore and mesoporous.Document 3 " know gorgeous and utilize template by original
Nano ordered mesoporous ceramic block material [D] the Changchun science and engineering of ancillary technique controllable preparation, 2011. " are prepared with sol-gal process
Mesoporous alumina powder, has then prepared meso-porous alumina ceramics by mesoporous powdered alumina into gel, injection molding sintering, when
It is 282m to have prepared specific surface area during 700 DEG C of sintering temperature2/ g, pore volume 0.57cm3/ g, average pore size 7.5nm, pressure
The meso-porous alumina ceramics that contracting intensity is 0.52Mpa.When sintering temperature is 1000 DEG C, the specific surface area of meso-porous alumina ceramics is
110m2/ g, pore volume 0.38cm3/ g, average pore size 12.0nm, compressive strength 1.23Mpa." nanometers of Wang Ding acute hearing is certainly for document 4
Assembling synthesizes big pore volume meso-porous alumina [J] Chinese sciences, 2009,39 (5):420-431. " utilized and received using sol-gal process
Rice self assembly mechanism is prepared for the big pore volume meso-porous alumina of secondary nanoassemble, its pore volume reaches 1.8-2.7ml/g, specific surface area
For 180-429m2/ g, average pore size 17-57nm, porosity reach 87%-93%." the organic bubble of Zhu Xinwen, the bright in the east of a river of document 5
A kind of foam impregnation technology --- economical and practical porous ceramics preparation process [J] silicates circular, 2000,03:45-51. " refer to
Go out sol-gal process is difficult to control pore-size distribution by adjusting the pH value of solution come adjustment aperture size and specific surface area, and raw
Low yield, process conditions are difficult to control, and are not suitable for large-scale production.Due in actual application, such as at the purification of sewage
Reason, needs specific surface area big in the discharge of tail gas, and intensity is high, and the good material of stability reaches catalysis as catalyst carrier
The purpose of purification, and sol-gal process prepares meso-porous alumina ceramics and not only needs to be prepared with reference to other methods, Er Qieqiang
Degree is difficult to meet actual application.
If preparing meso-porous alumina ceramics using powder sintering, method is simple, and cost is low, can realize that industrialization is big
Large-scale production, low-temperature sintering can save the energy again.Can be with adjustment apertures rate, specific surface area by the addition for adjusting binding agent
And bending strength.But meso-porous alumina ceramics were prepared with powder sintering there is presently no people, and how to adjust binding agent
A content problem making it under high specific surface area and porosity while there is higher intensity to be also the field.Therefore
It is to be solved as having in the area research that the ceramics of the meso-porous alumina with certain bending strength are prepared under high-specific surface area
Problem.
The content of the invention
For overcome it is existing in the prior art there is no powder sintering to prepare meso-porous alumina ceramics, and solve high ratio
There is the problem of higher intensity at the same time under surface area and porosity, the present invention proposes a kind of high specific surface area and mesoporous aluminium oxide
The preparation method of ceramics.
The present invention detailed process be：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared.The concentration of the aluminium dihydrogen phosphate aqueous solution is 4.5
~31.5%wt.
When the concentration of the aluminium dihydrogen phosphate aqueous solution need to be less than 31.5%wt, the di(2-ethylhexyl)phosphate using concentration as 31.5%wt
Hydrogen aluminum water solution mixes, and stir 10min and be uniformly mixed to obtain the phosphoric acid that concentration is 31.5%wt as raw material with deionized water
Dihydro aluminum water solution；The volume ratio of the aluminium dihydrogen phosphate aqueous solution and deionized water is 1~8:2~9；When the biphosphate
When the concentration of aluminum water solution need to be 31.5%wt, the aluminium dihydrogen phosphate aqueous solution that concentration is 31.5%wt is stirred into 10min and is obtained.
Step 2, the nanometer thin diaspore powder of wetting is prepared.By the biphosphate that 15ml concentration is 4.5~31.5%wt
Aluminum water solution is added drop-wise in the nanometer thin diaspore powder that weight is 30g, and the grinding stirring 20min in dropwise addition, is soaked
Nanometer thin diaspore powder.The granularity of the nanometer thin diaspore powder is 90~110nm, specific surface area 340m2/
g。
Step 3, press ceramic base substrate.Uniform nanometer thin diaspore powder will be soaked to be put into mould, powder is carried out
Pressure dual-side.Obtain ceramic body.
During the press ceramic base substrate, with<The rate of pressure rise pressurization of 1KN/s.When pressure reaches 381KN, pressurize 3min
After close press.
Step 4, ceramic body is dried.Obtained ceramic body is placed in drying baker, with the heating rate of 5 DEG C/min by
Room temperature is to 60 DEG C, the dry 2h at 60 DEG C, then is warming up to 120 DEG C by 60 DEG C with the heating rate of 5 DEG C/min, at 120 DEG C
When dry 2h.
Step 5, meso-porous alumina ceramics are fired.The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2
DEG C/programming rate of min by room temperature to 200 DEG C.After 200 DEG C, 500 are continuously heating to the programming rate of 5 DEG C/min
~800 DEG C, keep the temperature 2h.Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains mesoporous oxidation
Aluminium ceramics.
It is an object of the invention to when sintering temperature is less than 800 DEG C, produce a kind of specific surface area and be more than 100m2/ g, hole
Footpath is distributed between 2nm-50nm, and pore volume is located at 0.05-0.6cm3/ g, meso-porous alumina of the bending strength in 2Mpa-10Mpa
Ceramics.
The present invention prepares meso-porous alumina ceramics using aluminium dihydrogen phosphate as binding agent, using powder sintering.This method master
It is raw material with nanometer boehmite, aluminium dihydrogen phosphate is binding agent, and powder is molded with pressed disc method and sintering closes at low temperature
Into meso-porous alumina ceramics.The meso-porous alumina ceramics of this method synthesis are the accumulation construction ducts using nano-particle, are used
Powder shaping can have been saved the energy by pressed disc method according to required shape, while low-temperature sintering is actually prepared.
It is gel injection-moulding method to prepare the common method of meso-porous alumina ceramics at present.This method prepares meso-porous alumina pottery
Porcelain will prepare colloidal sol.The preparation of colloidal sol needs to use aluminium-alcohol salt (such as organo-aluminium alcoholate), template (such as P123) and other are organic molten
Agent, it is expensive.And pass through the specific surface areas of meso-porous alumina ceramics, pore volume, pore size prepared by colloidal sol be subject to it is a variety of because
The influence of element, such as：PH value after the addition of template, ageing time, calcining heat, reaction, makes its reaction process not easily-controllable
System.The especially size of pH value, the formation to meso-porous alumina pore volume, the size in aperture all have a great impact.And use nanometer
Boehmite does raw material, and preparing meso-porous alumina ceramics with powder sintering needs only to two variables of control, aluminium dihydrogen phosphate
The concentration of aqueous solution and the temperature of sintering.First, the bending strength of the good adhesive property increase material of phosphate dihydrogen aluminum solution,
The specific surface area and porosity of material can be controlled again by varying the addition of aluminium dihydrogen phosphate.It is 500 DEG C such as in sintering temperature,
The concentration of aluminium dihydrogen phosphate aqueous solution is respectively 4.5%wt, when 18.1%wt, 26.45%wt, prepared meso-porous alumina
The bending strength of ceramics is respectively 2.25Mpa, 3.0125MPa, 8.657Mpa, and specific surface area is respectively 326m2/g、
176.311m2/g、67.4238m2/ g, porosity are respectively 69.321%, 65.9457%, 63.1714%.Secondly, control is passed through
Temperature can also control the bending strength of meso-porous alumina ceramics, specific surface area and porosity.Such as in aluminium dihydrogen phosphate aqueous solution
Concentration be 18.1%wt, when sintering temperature is respectively 500 DEG C, 700 DEG C, the bending resistance of prepared meso-porous alumina ceramics is strong
Degree is respectively 3.30Mpa, 5.50Mpa, and specific surface area is respectively 176.311m2/g、106.673m2/ g, porosity are respectively
65.9457%, 67.1184%.The two conditions of the concentration and sintering temperature of aluminium dihydrogen phosphate aqueous solution are easy to control, and can
Realization significantly regulates and controls bending strength and specific surface area, overcomes other methods and prepares meso-porous alumina ceramics ratio not easy to control
The shortcomings that surface area and bending strength, at the same while changing the concentration and temperature of phosphate dihydrogen aluminum solution can obtain bending strength
It is obviously improved.It in the concentration of aluminium dihydrogen phosphate aqueous solution is 18.1%wt that attached drawing, which is, prepared when sintering temperature is 600 DEG C
The meso-porous alumina ceramics gone out.As shown in the pore size distribution curve 4 of attached drawing 4, the pore-size distribution of the meso-porous alumina ceramics of preparation
For 4~10nm, displacement-pressure curve 1 in attached drawing 1 shows that its bending strength can reach 5Mpa, and bending strength is
5.061Mpa, porosity 68.1263%.Pore volume curve 3 shown in attached drawing 3 shows prepared meso-porous alumina ceramics
Pore volume can reach 0.3cm3/g.The specific surface area of adsorption/desorption curve 2 shown in attached drawing 2 can reach 193.418m2/ g, with
The meso-porous alumina ceramic phase ratio prepared is known in present domestic literature, under identical specific surface area, bending strength by
1.05Mpa has brought up to 5Mpa.
This invention simplifies the technique for preparing meso-porous alumina ceramics so that the production cycle shortens half, can realize rule
The efficient production of modelling.And the nanometer boehmite system industrially that the feedstock particle size of this method is 100nm
Standby technology is more mature, existing a variety of preparation methods.
Brief description of the drawings
Fig. 1 is the meso-porous alumina ceramics bending strength curve that the present invention prepares；
Fig. 2 is the meso-porous alumina ceramics desorption adsorption curve that the present invention prepares；
Fig. 3 is the pore volume curve for the meso-porous alumina ceramics that the present invention prepares；
Fig. 4 is the meso-porous alumina ceramics pore size distribution curve that the present invention prepares；
Fig. 5 is the flow chart of the present invention.In figure：
1. displacement-pressure curve；2. adsorption/desorption curve；3. pore volume curve；4. pore size distribution curve.
Embodiment
Embodiment one：
The present embodiment is a kind of method that meso-porous alumina ceramics are prepared with powder sintering, and detailed process is：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared.In the present embodiment, required aluminium dihydrogen phosphate is water-soluble
The concentration of liquid is 4.5%wt.
During preparation, the aluminium dihydrogen phosphate aqueous solution using concentration as 31.5%wt is used as raw material.By the aluminium dihydrogen phosphate
Aqueous solution presses 1 with deionized water:9 volume ratio mixing, and 10min is stirred with glass bar, it is uniformly mixed, that is, is made dense
Spend the aluminium dihydrogen phosphate aqueous solution for 4.5%wt.
Step 2, the nanometer thin diaspore powder of wetting is prepared.The nanometer thin diaspore powder that weight is 30g is put into and is ground
In alms bowl.Take the aluminium dihydrogen phosphate aqueous solution that 15ml concentration is 4.5%wt.The molten water drop of the aluminium dihydrogen phosphate is added in described receive
In rice boehmite powder, and the grinding stirring 20min in dropwise addition, make nanometer thin diaspore powder and aluminium dihydrogen phosphate aqueous solution
It is uniformly mixed, the nanometer thin diaspore powder soaked.The granularity of the nanometer thin diaspore powder for 90~
110nm, specific surface area 340m2/g。
The nanometer boehmite is the industrial raw material that Zhong Shengzhen spaces company provides.
Step 3, press ceramic base substrate.Uniform nanometer thin diaspore powder will be soaked to be placed on a diameter of 90mm, be highly
60mm, and in No. 45 steel cylindrical type moulds by quenching, pressure dual-side is carried out to powder.During pressurization, with<The boosting of 1KN/s
Speed is pressurizeed.When pressure reaches the i.e. 60Mpa of 381KN, press is closed after pressurize 3min.Taking out the surface diameter suppressed is
90mm, thickness are the patty ceramic body of 3~4mm.
Step 4, ceramic body is dried.The ceramic body pressed in step 3 is placed in drying baker, with the liter of 5 DEG C/min
Warm speed, to 60 DEG C, dries 2h by room temperature at 60 DEG C, then is warming up to 120 DEG C by 60 DEG C with the programming rate of 5 DEG C/min,
2h is dried at 120 DEG C, the ceramic body dried.
Step 5, meso-porous alumina ceramics are fired.The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2
DEG C/programming rate of min by room temperature to 200 DEG C.After 200 DEG C, 500 are continuously heating to the programming rate of 5 DEG C/min
DEG C, keep the temperature 2h.Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains meso-porous alumina pottery
Porcelain.
Embodiment two：
The present embodiment is a kind of method that meso-porous alumina ceramics are prepared with powder sintering, and detailed process is：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared.In the present embodiment, required aluminium dihydrogen phosphate is water-soluble
The concentration of liquid is 18.1%wt.
During preparation, the aluminium dihydrogen phosphate aqueous solution using concentration as 31.5%wt is used as raw material.By the aluminium dihydrogen phosphate
Aqueous solution presses 5 with deionized water:5 volume ratio mixing, and 10min is stirred with glass bar, it is uniformly mixed, that is, is made dense
Spend the aluminium dihydrogen phosphate aqueous solution for 18.1%wt.
Step 2, the nanometer thin diaspore powder of wetting is prepared.The nanometer thin diaspore powder that weight is 30g is put into and is ground
In alms bowl.Take the aluminium dihydrogen phosphate aqueous solution that 15ml concentration is 18.1%wt.The molten water drop of the aluminium dihydrogen phosphate is added in described
In nanometer thin diaspore powder, and the grinding stirring 20min in dropwise addition, make nanometer thin diaspore powder and aluminium dihydrogen phosphate water-soluble
Liquid is uniformly mixed, the nanometer thin diaspore powder soaked.The granularity of the nanometer thin diaspore powder for 90~
110nm, specific surface area 340m2/g。
The nanometer boehmite is the industrial raw material that Zhong Shengzhen spaces company provides.
Step 3, press ceramic base substrate.Uniform nanometer thin diaspore powder will be soaked to be placed on a diameter of 90mm, be highly
60mm, and in No. 45 steel cylindrical type moulds by quenching, pressure dual-side is carried out to powder.During pressurization, with<The boosting of 1KN/s
Speed is pressurizeed.When pressure reaches the i.e. 60Mpa of 381KN, press is closed after pressurize 3min.Taking out the surface diameter suppressed is
90mm, thickness are the patty ceramic body of 3~4mm.
Step 4, ceramic body is dried.The ceramic body pressed in step 3 is placed in drying baker with the heating of 5 DEG C/min
Speed, to 60 DEG C, dries 2h by room temperature at 60 DEG C, then is warming up to 120 DEG C by 60 DEG C with the heating rate of 5 DEG C/min,
2h is dried at 120 DEG C.
Step 5, meso-porous alumina ceramics are fired.The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2
DEG C/programming rate of min by room temperature to 200 DEG C.After 200 DEG C, 600 are continuously heating to the programming rate of 5 DEG C/min
DEG C, keep the temperature 2h.Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains meso-porous alumina pottery
Porcelain.
Embodiment three：
The present embodiment is a kind of method that meso-porous alumina ceramics are prepared with powder sintering, and detailed process is：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared.In the present embodiment, required aluminium dihydrogen phosphate is water-soluble
The concentration of liquid is 4.5%wt.
During preparation, the aluminium dihydrogen phosphate aqueous solution using concentration as 31.5%wt is used as raw material.By the aluminium dihydrogen phosphate
Aqueous solution presses 1 with deionized water:9 volume ratio mixing, and 10min is stirred with glass bar, it is uniformly mixed, that is, is made dense
Spend the aluminium dihydrogen phosphate aqueous solution for 4.5%wt.
Step 2, the nanometer thin diaspore powder of wetting is prepared.The nanometer thin diaspore powder that weight is 30g is put into and is ground
In alms bowl.Take the aluminium dihydrogen phosphate aqueous solution that 15ml concentration is 4.5%wt.The molten water drop of the aluminium dihydrogen phosphate is added in described receive
In rice boehmite powder, and the grinding stirring 20min in dropwise addition, make nanometer thin diaspore powder and aluminium dihydrogen phosphate aqueous solution
It is uniformly mixed, the nanometer thin diaspore powder soaked.The granularity of the nanometer thin diaspore powder for 90~
110nm, specific surface area 340m2/g。
The nanometer boehmite is the industrial raw material that Zhong Shengzhen spaces company provides.
Step 3, press ceramic base substrate.Uniform nanometer thin diaspore powder will be soaked to be placed on a diameter of 90mm, be highly
60mm, and in No. 45 steel cylindrical type moulds by quenching, pressure dual-side is carried out to powder.During pressurization, with<The boosting of 1KN/s
Speed is pressurizeed.When pressure reaches the i.e. 60Mpa of 381KN, press is closed after pressurize 3min.Taking out the surface diameter suppressed is
90mm, thickness are the patty ceramic body of 3~4mm.
Step 4, ceramic body is dried.The ceramic body pressed in step 3 is placed in drying baker with the heating of 5 DEG C/min
Speed, to 60 DEG C, dries 2h by room temperature at 60 DEG C, then is warming up to 120 DEG C by 60 DEG C with the heating rate of 5 DEG C/min,
2h is dried at 120 DEG C.
Step 5, meso-porous alumina ceramics are fired.The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2
DEG C/programming rate of min by room temperature to 200 DEG C.After 200 DEG C, 800 are continuously heating to the programming rate of 5 DEG C/min
DEG C, keep the temperature 2h.Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains meso-porous alumina pottery
Porcelain.
Example IV：
The present embodiment is a kind of method that meso-porous alumina ceramics are prepared with powder sintering, and detailed process is：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared.In the present embodiment, required aluminium dihydrogen phosphate is water-soluble
The concentration of liquid is 26.45%wt.
During preparation, the aluminium dihydrogen phosphate aqueous solution using concentration as 31.5%wt is used as raw material.By the aluminium dihydrogen phosphate
Aqueous solution presses 8 with deionized water:2 volume ratio mixing, and 10min is stirred with glass bar, it is uniformly mixed, that is, is made dense
Spend the aluminium dihydrogen phosphate aqueous solution for 26.45%wt.
Step 2, the nanometer thin diaspore powder of wetting is prepared.The nanometer thin diaspore powder that weight is 30g is put into and is ground
In alms bowl.Take the aluminium dihydrogen phosphate aqueous solution that 15ml concentration is 26.45%wt.The molten water drop of the aluminium dihydrogen phosphate is added in described
In nanometer thin diaspore powder, and the grinding stirring 20min in dropwise addition, make nanometer thin diaspore powder and aluminium dihydrogen phosphate water-soluble
Liquid is uniformly mixed, the nanometer thin diaspore powder soaked.The granularity of the nanometer thin diaspore powder for 90~
110nm, specific surface area 340m2/g。
The nanometer boehmite is the industrial raw material that Zhong Shengzhen spaces company provides.
Step 3, press ceramic base substrate.Uniform nanometer thin diaspore powder will be soaked to be placed on a diameter of 90mm, be highly
60mm, and in No. 45 steel cylindrical type moulds by quenching, pressure dual-side is carried out to powder.During pressurization, with<The boosting of 1KN/s
Speed is pressurizeed.When pressure reaches the i.e. 60Mpa of 381KN, press is closed after pressurize 3min.Taking out the surface diameter suppressed is
90mm, thickness are the patty ceramic body of 3~4mm.
Step 4, ceramic body is dried.The ceramic body pressed in step 3 is placed in drying baker with the heating of 5 DEG C/min
Speed, to 60 DEG C, dries 2h by room temperature at 60 DEG C, then is warming up to 120 DEG C by 60 DEG C with the heating rate of 5 DEG C/min,
2h is dried at 120 DEG C.
Step 5, meso-porous alumina ceramics are fired.The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2
DEG C/programming rate of min by room temperature to 200 DEG C.After 200 DEG C, 700 are continuously heating to the programming rate of 5 DEG C/min
DEG C, keep the temperature 2h.Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains meso-porous alumina pottery
Porcelain.
Embodiment five：
The present embodiment is a kind of method that meso-porous alumina ceramics are prepared with powder sintering, and detailed process is：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared.In the present embodiment, required aluminium dihydrogen phosphate is water-soluble
The concentration of liquid is 31.5%wt.
During preparation, the concentration of used aluminium dihydrogen phosphate aqueous solution stoste is 31.5%wt, and so there is no need to use deionized water
Dilution.The aluminium dihydrogen phosphate aqueous solution for taking 15ml concentration to be 31.5%wt is put into beaker, and 10min is stirred with glass bar.
Step 2, the nanometer thin diaspore powder of wetting is prepared.The nanometer thin diaspore powder that weight is 30g is put into and is ground
In alms bowl.Take the aluminium dihydrogen phosphate aqueous solution that 15ml concentration is 31.5%wt.The molten water drop of the aluminium dihydrogen phosphate is added in described
In nanometer thin diaspore powder, and the grinding stirring 20min in dropwise addition, make nanometer thin diaspore powder and aluminium dihydrogen phosphate water-soluble
Liquid is uniformly mixed, the nanometer thin diaspore powder soaked.The granularity of the nanometer thin diaspore powder for 90~
110nm, specific surface area 340m2/g
The nanometer boehmite is the industrial raw material that Zhong Shengzhen spaces company provides.
Step 3, press ceramic base substrate.Uniform nanometer thin diaspore powder will be soaked to be placed on a diameter of 90mm, be highly
60mm, and in No. 45 steel cylindrical type moulds by quenching, pressure dual-side is carried out to powder.During pressurization, with<The boosting of 1KN/s
Speed is pressurizeed.When pressure reaches the i.e. 60Mpa of 381KN, press is closed after pressurize 3min.Taking out the surface diameter suppressed is
90mm, thickness are the patty ceramic body of 3~4mm.
Step 4, ceramic body is dried.The ceramic body pressed in step 3 is placed in drying baker with the heating of 5 DEG C/min
Speed, to 60 DEG C, dries 2h by room temperature at 60 DEG C, then is warming up to 120 DEG C by 60 DEG C with the heating rate of 5 DEG C/min,
2h is dried at 120 DEG C.
Step 5, meso-porous alumina ceramics are fired.The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2
DEG C/programming rate of min by room temperature to 200 DEG C.After 200 DEG C, 500 are continuously heating to the programming rate of 5 DEG C/min
DEG C, keep the temperature 2h.Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains meso-porous alumina pottery
Porcelain.
Claims (4)
1. a kind of preparation method of high specific surface area and mesoporous aluminium oxide ceramics, it is characterised in that detailed process is：
Step 1, the aluminium dihydrogen phosphate aqueous solution of various concentrations is prepared：The concentration of the aluminium dihydrogen phosphate aqueous solution for 4.5~
31.5%wt；
Step 2, the nanometer thin diaspore powder of wetting is prepared：By the aluminium dihydrogen phosphate water that 15ml concentration is 4.5~31.5%wt
Solution is added drop-wise in the nanometer thin diaspore powder that weight is 30g, and the grinding stirring 20min in dropwise addition, and what is soaked receives
Rice boehmite powder；
Step 3, press ceramic base substrate：Uniform nanometer thin diaspore powder will be soaked to be put into mould, powder is carried out two-sided
Pressurization；Obtain ceramic body；
Step 4, ceramic body is dried：Obtained ceramic body is placed in drying baker, with the heating rate of 5 DEG C/min by room temperature
60 DEG C are warming up to, the dry 2h at 60 DEG C, then 120 DEG C are warming up to by 60 DEG C with the heating rate of 5 DEG C/min, done at 120 DEG C
Dry 2h；
Step 5, meso-porous alumina ceramics are fired：The ceramic body of drying is put into Muffle furnace carry out it is normal pressure-sintered：With 2 DEG C/
The programming rate of min is by room temperature to 200 DEG C；After 200 DEG C, 500 are continuously heating to the programming rate of 5 DEG C/min~
800 DEG C, keep the temperature 2h；Power supply is closed after insulation, is taken out after burned ceramics are cooled to room temperature, that is, obtains meso-porous alumina
Ceramics.
2. the preparation method of high specific surface area and mesoporous aluminium oxide ceramics as claimed in claim 1, it is characterised in that when the phosphoric acid
When the concentration of dihydro aluminum water solution need to be less than 31.5%wt, the aluminium dihydrogen phosphate aqueous solution using concentration as 31.5%wt is used as original
Material, mixes with deionized water, and stirs 10min and be uniformly mixed, and obtains the aluminium dihydrogen phosphate aqueous solution of various concentrations；The phosphoric acid
The volume ratio of dihydro aluminum water solution and deionized water is 1~8:2~9；When the concentration of the aluminium dihydrogen phosphate aqueous solution need to be
During 31.5%wt, the aluminium dihydrogen phosphate aqueous solution that concentration is 31.5%wt is stirred what 10min was obtained.
3. the preparation method of high specific surface area and mesoporous aluminium oxide ceramics as claimed in claim 1, it is characterised in that the compacting pottery
During porcelain billet body, with<The rate of pressure rise pressurization of 1KN/s；When pressure reaches 381KN, press is closed after pressurize 3min.
4. the preparation method of high specific surface area and mesoporous aluminium oxide ceramics as claimed in claim 1, it is characterised in that the nanometer
The granularity of boehmite powder is 90~110nm, specific surface area 340m2/g。
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| CN104129983A (en) * | 2014-07-07 | 2014-11-05 | 山东理工大学 | High-strength block-shaped porous magnesia-alumina spinel nano-ceramic preparation method |
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