CN107434426A - A kind of mullite multi-stage porous ceramics and preparation method thereof - Google Patents

A kind of mullite multi-stage porous ceramics and preparation method thereof Download PDF

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Publication number
CN107434426A
CN107434426A CN201710601380.8A CN201710601380A CN107434426A CN 107434426 A CN107434426 A CN 107434426A CN 201710601380 A CN201710601380 A CN 201710601380A CN 107434426 A CN107434426 A CN 107434426A
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mullite
stage porous
porous ceramics
powder
preparation
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张海军
葛胜涛
毕玉保
张少伟
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Wuhan University of Science and Engineering WUSE
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
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Abstract

The present invention relates to a kind of mullite multi-stage porous ceramics and preparation method thereof.Its technical scheme is：By the mullite powder of 96 ~ 100 parts of quality and the nano-calcium carbonate powder ball milling of 0 ~ 4 part of quality, ball milling powder is obtained；Stabilizer is soaked in deionized water, stirred, obtained solution；Dispersant and the ball milling powder are added in solution, stirring, ceramic slurry is made；Foaming agent is added into the ceramic slurry, is stirred, foamed slurry is made；The foamed slurry is injected in mould, the in-situ solidifying under the conditions of 10 ~ 60 DEG C, the demoulding, mullite multi-stage porous ceramic body is made；By the mullite multi-stage porous ceramic blank drying, 1 ~ 6h is calcined under the conditions of 1300 ~ 1550 DEG C, mullite multi-stage porous ceramics are made.The present invention has the characteristics of synthesis technique is simple, easily controllable, pollution is small low with production cost；Prepared mullite multi-stage porous ceramics strength is high, aperture is small and is evenly distributed, thermal conductivity factor is low and suitable for large-scale production.

Description

A kind of mullite multi-stage porous ceramics and preparation method thereof
Technical field
The invention belongs to multi-stage porous ceramic technology field.More particularly to a kind of mullite multi-stage porous ceramics and its preparation side Method.
Background technology
Multi-stage porous ceramics have pore structure diversity, porosity height, specific surface area is big, thermal conductivity factor is low, bulk density is small With the excellent specific property such as chemical property is stable, liquid chromatogram separation, gas liquid filtering, catalyst carrier, high temperature insulating material, The field such as ultracapacitor and bioengineering has a wide range of applications and potential application prospect.
At present, the preparation method of mullite multi-stage porous ceramics mainly has：Sol-gel process, molten-salt growth method, foam impregnation method and Granulation mass area method etc..Although these methods respectively have advantage, some shortcomings are wherein still suffered from：If sol-gel process is mostly with alcohol Salt is raw material, expensive；The hydrolysis rate of alkoxide is different simultaneously, complex technical process, whard to control and preparation cost It is high." a kind of mullite porous ceramic and preparation method thereof "（CN104446623A）Using mullite powder as raw material, it is prepared for not Carry out stone porous ceramics, mullite porous ceramic base substrate hardening time length, low intensity and the demoulding prepared by this method is difficult, and sinters Obtained ceramics sample low intensity, aperture is big and thermal conductivity factor is big.Though molten-salt growth method can prepare uniform pore diameter distribution at low temperature Mullite multi-stage porous ceramics, but the volatilization of fuse salt seriously endangers health and pollutes environment, and the aperture of products obtained therefrom Greatly, impurity content height and low yield, it is expensive so as to cause.Mullite multi-stage porous ceramics strength prepared by foam impregnation method Low, the shape in hole is by template contral, and environment is easily polluted in the burning of foam organic formwork.Mullite prepared by granulation mass area method Multi-stage porous ceramics porosity is too low, poor-performing.
In summary, deficiency existing for existing mullite multi-stage porous ceramics processing is：Complex process and not easily-controllable System, organic matter dosage is big, environmental pollution is serious and production cost is high etc., limits mullite multi-stage porous ceramics scale in the industry The production and application of change.
The content of the invention
It is contemplated that overcome the deficiencies in the prior art, it is therefore an objective to provide a kind of synthesis technique it is simple, it is easily controllable, pollution The preparation method of the small mullite multi-stage porous ceramics low with production cost；The mullite multi-stage porous ceramics prepared using this method are strong Degree is high, aperture is small and is evenly distributed, thermal conductivity factor is low and suitable for large-scale production.
To achieve the above object, the preparation process of the technical solution adopted by the present invention is：
Step 1: the nano-calcium carbonate powder of the mullite powder of 96 ~ 100 parts of quality and 0 ~ 4 part of quality is placed in ball mill, 180 ~ 240min of ball milling, produce ball milling powder.
Step 2: by stabilizer: the mass ratio of deionized water is（0.001~0.006）: 1, by the stabilizer go from 12 ~ 24h is soaked in sub- water, stirs 10 ~ 20min, obtained solution.
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.003~0.03）∶（2~3.6）∶ 1, the dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, ceramic slurry is made.
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.00025~0.012）: 1, to the ceramic slurry The foaming agent is added in material, stirs 5 ~ 30min, foamed slurry is made.
Step 5: the foamed slurry is injected in mould, in-situ solidifying 1 ~ 6 hour under the conditions of 10 ~ 60 DEG C, the demoulding, Mullite multi-stage porous ceramic body is made.
Step 6: by the mullite multi-stage porous ceramic blank drying, 1 ~ 6h, system are calcined under the conditions of 1300 ~ 1550 DEG C Obtain mullite multi-stage porous ceramics.
Median≤10 μm of the mullite powder, 3Al2O3·2SiO2Content >=98wt%.
The median of the nano-calcium carbonate is≤150nm, CaCO3Content >=98wt%.
The stabilizer is carboxymethyl cellulose or is hydroxypropyl methyl cellulose, and the stabilizer is technical pure or is point Analyse pure.
The dispersant is the copolymer of isobutyiene-maieic anhydride or is ammonium polyacrylate, and the dispersant is technical pure It is or pure to analyze.
Due to using above-mentioned technical scheme, the present invention has the positive effect that compared with prior art：
1st, stabilizer of the present invention is carboxymethyl cellulose or is hydroxypropyl methyl cellulose, safe and non-toxic；Adopted Dispersant is the copolymer of isobutyiene-maieic anhydride or is ammonium polyacrylate, and based on C, H and O, N contains the dispersant Amount is very low, small to operating personnel and environmental hazard.
2nd, the stabilizer that uses of the present invention and the total amount of dispersant and the quality of deionized water for（0.004~0.036）: 1, Content is relatively low, therefore production cost is low, suitable for large-scale production.
3rd, mullite powder and nano-calcium carbonate powder ball milling are obtained ball milling powder by the present invention；By dispersant and ball milling powder Body is added in solution, adds foaming agent, and foamed slurry is made, is then injected into mould, in-situ solidifying, is calcined, and is made and is not come Stone multi-stage porous ceramics, technique are simple.
4th, the present invention produces CO by nano-calcium carbonate pyrolytic2Gas, aperture is produced inside ceramics, pass through foaming Technique produces macropore inside ceramics, and mullite multi-stage porous ceramics are made.The intensity of prepared mullite multi-stage porous ceramics is high, Aperture is small and is evenly distributed, and thermal conductivity factor is low.
Mullite multi-stage porous ceramics prepared by the present invention are after testing：Porosity is 62 ~ 79%；Compressive resistance is 5 ~ 30Mpa； Average pore size is 0.7 ~ 203 μm；Thermal conductivity factor is 0.11 ~ 0.29W/ (mK).
Therefore, the present invention has the characteristics of synthesis technique is simple, easily controllable, pollution is small low with production cost；It is prepared Mullite multi-stage porous ceramics strength it is high, aperture is small and is evenly distributed, thermal conductivity factor is low and suitable for large-scale production.
Brief description of the drawings
Fig. 1 is a kind of SEM figures of mullite multi-stage porous ceramics prepared by the present invention.
Embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain System.
It is first that the material Unify legislation involved by present embodiment is as follows to avoid repeating, it is no longer superfluous in embodiment State：
Median≤10 μm of the mullite powder, 3Al2O3·2SiO2Content >=98wt%.
The median of the nano-calcium carbonate is≤150nm, CaCO3Content >=98wt%.
The stabilizer is carboxymethyl cellulose or is hydroxypropyl methyl cellulose, and the stabilizer is technical pure or is point Analyse pure.
The dispersant is the copolymer of isobutyiene-maieic anhydride or is ammonium polyacrylate, and the dispersant is technical pure It is or pure to analyze.
Embodiment 1
A kind of mullite multi-stage porous ceramics and preparation method thereof.Preparation method is described in the present embodiment：
Step 1: the nano-calcium carbonate powder of the mullite powder of 96 ~ 97 parts of quality and 3 ~ 4 parts of quality is placed in ball mill, 180 ~ 240min of ball milling, produce ball milling powder.
Step 2: by stabilizer: the mass ratio of deionized water is（0.001~0.002）: 1, by the stabilizer go from 12 ~ 24h is soaked in sub- water, stirs 10 ~ 20min, obtained solution.
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.003~0.01）∶（2~2.8）∶ 1, the dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, ceramic slurry is made.
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.01~0.012）: 1, into the ceramic slurry The foaming agent is added, stirs 5 ~ 30min, foamed slurry is made.
Step 5: the foamed slurry is injected in mould, in-situ solidifying 1 ~ 3 hour under the conditions of 40 ~ 60 DEG C, the demoulding, Mullite multi-stage porous ceramic body is made.
Step 6: by the mullite multi-stage porous ceramic blank drying, 4 ~ 6h, system are calcined under the conditions of 1300 ~ 1400 DEG C Obtain mullite multi-stage porous ceramics.
In the present embodiment：The stabilizer is carboxymethyl cellulose；The dispersant is the copolymerization of isobutyiene-maieic anhydride Thing.
Mullite multi-stage porous ceramics prepared by the present invention are after testing：Porosity is 74 ~ 79%；Compressive resistance is 5 ~ 9Mpa；It is flat Equal aperture is 0.7 ~ 134 μm；Thermal conductivity factor is 0.11 ~ 0.14W/ (mK).
Embodiment 2
A kind of mullite multi-stage porous ceramics and preparation method thereof.Preparation method is described in the present embodiment：
Step 1: the nano-calcium carbonate powder of the mullite powder of 97 ~ 98 parts of quality and 2 ~ 3 parts of quality is placed in ball mill, 180 ~ 240min of ball milling, produce ball milling powder.
Step 2: by stabilizer: the mass ratio of deionized water is（0.002~0.003）: 1, by the stabilizer go from 12 ~ 24h is soaked in sub- water, stirs 10 ~ 20min, obtained solution.
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.01~0.015）∶（2.2~3.0） : 1, the dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, ceramic slurry is made.
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.008~0.010）: 1, to the ceramic slurry It is middle to add the foaming agent, 5 ~ 30min is stirred, foamed slurry is made.
Step 5: the foamed slurry is injected in mould, in-situ solidifying 2 ~ 4 hours under the conditions of 30 ~ 50 DEG C, the demoulding, Mullite multi-stage porous ceramic body is made.
Step 6: by the mullite multi-stage porous ceramic blank drying, 3 ~ 5h, system are calcined under the conditions of 1330 ~ 1430 DEG C Obtain mullite multi-stage porous ceramics.
In the present embodiment：The stabilizer is carboxymethyl cellulose；The dispersant is ammonium polyacrylate.
Mullite multi-stage porous ceramics prepared by the present invention are after testing：Porosity is 72 ~ 76%；Compressive resistance is 7 ~ 13Mpa； Average pore size is 3 ~ 156 μm；Thermal conductivity factor is 0.13 ~ 0.18W/ (mK).
Embodiment 3
A kind of mullite multi-stage porous ceramics and preparation method thereof.Preparation method is described in the present embodiment：
Step 1: the nano-calcium carbonate powder of the mullite powder of 98 ~ 99 parts of quality and 1 ~ 2 part of quality is placed in ball mill, 180 ~ 240min of ball milling, produce ball milling powder.
Step 2: by stabilizer: the mass ratio of deionized water is（0.003~0.004）: 1, by the stabilizer go from 12 ~ 24h is soaked in sub- water, stirs 10 ~ 20min, obtained solution.
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.015~0.02）∶（2.4~3.2） : 1, the dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, ceramic slurry is made.
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.005~0.008）: 1, to the ceramic slurry It is middle to add the foaming agent, 5 ~ 30min is stirred, foamed slurry is made.
Step 5: the foamed slurry is injected in mould, in-situ solidifying 3 ~ 5 hours under the conditions of 20 ~ 40 DEG C, the demoulding, Mullite multi-stage porous ceramic body is made.
Step 6: by the mullite multi-stage porous ceramic blank drying, 2 ~ 4h, system are calcined under the conditions of 1370 ~ 1470 DEG C Obtain mullite multi-stage porous ceramics.
In the present embodiment：The stabilizer is hydroxypropyl methyl cellulose；The dispersant is isobutyiene-maieic anhydride Copolymer.
Mullite multi-stage porous ceramics prepared by the present invention are after testing：Porosity is 69 ~ 75%；Compressive resistance is 11 ~ 17Mpa； Average pore size is 17 ~ 189 μm；Thermal conductivity factor is 0.16 ~ 0.20W/ (mK).
Embodiment 4
A kind of mullite multi-stage porous ceramics and preparation method thereof.Preparation method is described in the present embodiment：
Step 1: the nano-calcium carbonate powder of the mullite powder of 99 ~ 99.9 parts of quality and 0.1 ~ 1 part of quality is placed in ball mill In, 180 ~ 240min of ball milling, produce ball milling powder.
Step 2: by stabilizer: the mass ratio of deionized water is（0.004~0.005）: 1, by the stabilizer go from 12 ~ 24h is soaked in sub- water, stirs 10 ~ 20min, obtained solution.
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.020~0.025）∶（2.6~ 3.4）: 1, the dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, ceramic slurry is made.
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.001~0.005）: 1, to the ceramic slurry It is middle to add the foaming agent, 5 ~ 30min is stirred, foamed slurry is made.
Step 5: the foamed slurry is injected in mould, in-situ solidifying 4 ~ 6 hours under the conditions of 10 ~ 30 DEG C, the demoulding, Mullite multi-stage porous ceramic body is made.
Step 6: by the mullite multi-stage porous ceramic blank drying, 1 ~ 3h, system are calcined under the conditions of 1410 ~ 1510 DEG C Obtain mullite multi-stage porous ceramics.
In the present embodiment：The stabilizer is hydroxypropyl methyl cellulose；The dispersant is ammonium polyacrylate.
Mullite multi-stage porous ceramics prepared by the present invention are after testing：Porosity is 67 ~ 73%；Compressive resistance is 16 ~ 23Mpa； Average pore size is 32 ~ 198 μm；Thermal conductivity factor is 0.19 ~ 0.25W/ (mK).
Embodiment 5
A kind of mullite multi-stage porous ceramics and preparation method thereof.Preparation method is described in the present embodiment：
Step 1: the mullite powder of 100 parts of quality is placed in ball mill, 180 ~ 240min of ball milling, ball milling powder is produced.
Step 2: by stabilizer: the mass ratio of deionized water is（0.005~0.006）: 1, by the stabilizer go from 12 ~ 24h is soaked in sub- water, stirs 10 ~ 20min, obtained solution.
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.025~0.03）∶（2.8~3.6） : 1, the dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, ceramic slurry is made.
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.00025~0.001）: 1, to the ceramic slurry The foaming agent is added in material, stirs 5 ~ 30min, foamed slurry is made.
Step 5: the foamed slurry is injected in mould, in-situ solidifying 2.5 ~ 4.5 hours under the conditions of 25 ~ 45 DEG C, take off Mould, mullite multi-stage porous ceramic body is made.
Step 6: by the mullite multi-stage porous ceramic blank drying, calcine 3.5 under the conditions of 1450 ~ 1550 DEG C ~ 5.5h, mullite multi-stage porous ceramics are made.
In the present embodiment：The stabilizer is carboxymethyl cellulose；The dispersant is the copolymerization of isobutyiene-maieic anhydride Thing.
Mullite multi-stage porous ceramics prepared by the present invention are after testing：Porosity is 62 ~ 68%；Compressive resistance is 22 ~ 30Mpa； Average pore size is 51 ~ 203 μm；Thermal conductivity factor is 0.24 ~ 0.29W/ (mK).
Present embodiment has the positive effect that compared with prior art：
1st, stabilizer is carboxymethyl cellulose or is hydroxypropyl methyl cellulose used by present embodiment, safe nothing Poison；Used dispersant is the copolymer of isobutyiene-maieic anhydride or is ammonium polyacrylate, the dispersant using C, H and O as Main, N content is very low, small to operating personnel and environmental hazard.
2nd, present embodiment uses stabilizer and the total amount of dispersant and the quality of deionized water for（0.004~ 0.036）: 1, content is relatively low, therefore production cost is low, suitable for large-scale production.
3rd, mullite powder and nano-calcium carbonate powder ball milling are obtained ball milling powder by present embodiment；By dispersant Added with ball milling powder in solution, add foaming agent, foamed slurry is made, is then injected into mould, in-situ solidifying, calcined, Mullite multi-stage porous ceramics are made, technique is simple.
4th, present embodiment produces CO by nano-calcium carbonate pyrolytic2Gas, aperture is produced inside ceramics, Macropore is produced inside ceramics by foam process, mullite multi-stage porous ceramics are made as shown in figure 1, Fig. 1 is prepared for embodiment 1 A kind of mullite multi-stage porous ceramics SEM figure, as can be seen from Figure 1：The aperture of made product is small and is evenly distributed.
Mullite multi-stage porous ceramics prepared by present embodiment are after testing：Porosity is 62 ~ 79%；Compressive resistance is 5 ~30Mpa；Average pore size is 0.7 ~ 203 μm；Thermal conductivity factor is 0.11 ~ 0.29W/ (mK).
Therefore, present embodiment has that synthesis technique is simple, easily controllable, the small spy low with production cost of pollution Point；Prepared mullite multi-stage porous ceramics strength is high, aperture is small and is evenly distributed, thermal conductivity factor is low and suitable for scale metaplasia Production.

Claims (6)

1. the preparation method of a kind of mullite multi-stage porous ceramics, it is characterised in that be the step of the preparation method：
Step 1: the nano-calcium carbonate powder of the mullite powder of 96 ~ 100 parts of quality and 0 ~ 4 part of quality is placed in ball mill, 180 ~ 240min of ball milling, produce ball milling powder；
Step 2: by stabilizer: the mass ratio of deionized water is（0.001~0.006）: 1, by the stabilizer in deionized water 12 ~ 24h of middle immersion, stir 10 ~ 20min, obtained solution；
Step 3: by dispersant: the ball milling powder: the mass ratio of deionized water is（0.003~0.03）∶（2~3.6）: 1, will The dispersant and the ball milling powder are added in the solution, stir 10 ~ 30min, and ceramic slurry is made；
Step 4: by foaming agent: the volume ratio of the ceramic slurry is（0.00025~0.012）: 1, into the ceramic slurry The foaming agent is added, stirs 5 ~ 30min, foamed slurry is made；
Step 5: the foamed slurry is injected in mould, in-situ solidifying 1 ~ 6 hour under the conditions of 10 ~ 60 DEG C, it is stripped, is made Mullite multi-stage porous ceramic body；
Step 6: by the mullite multi-stage porous ceramic blank drying, 1 ~ 6h is calcined under the conditions of 1300 ~ 1550 DEG C, is made not Carry out stone multi-stage porous ceramics.
2. the preparation method of mullite multi-stage porous ceramics according to claim 1, it is characterised in that the mullite powder Median≤10 μm, 3Al2O3·2SiO2Content >=98wt%.
3. the preparation method of mullite multi-stage porous ceramics according to claim 1, it is characterised in that the nano-calcium carbonate Median is≤150nm, CaCO3Content >=98wt%.
4. the preparation method of mullite multi-stage porous ceramics according to claim 1, it is characterised in that the stabilizer is carboxylic first Base cellulose is hydroxypropyl methyl cellulose, and the stabilizer is technical pure or is that analysis is pure.
5. the preparation method of mullite multi-stage porous ceramics according to claim 1, it is characterised in that the dispersant is isobutyl The copolymer of alkene-maleic anhydride is ammonium polyacrylate, and the dispersant is technical pure or is that analysis is pure.
6. a kind of mullite multi-stage porous ceramics, it is characterised in that the mullite multi-stage porous ceramics are according to claim 1 ~ 5 Any one of mullite multi-stage porous ceramics preparation method prepared by mullite multi-stage porous ceramics.
CN201710601380.8A 2017-07-21 2017-07-21 A kind of mullite multi-stage porous ceramics and preparation method thereof Withdrawn CN107434426A (en)

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Application publication date: 20171205