CN101913885A - Method for processing sols of alumina refractory particles - Google Patents
Method for processing sols of alumina refractory particles Download PDFInfo
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- CN101913885A CN101913885A CN 201010230998 CN201010230998A CN101913885A CN 101913885 A CN101913885 A CN 101913885A CN 201010230998 CN201010230998 CN 201010230998 CN 201010230998 A CN201010230998 A CN 201010230998A CN 101913885 A CN101913885 A CN 101913885A
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- magnesium
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- alumina refractory
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Abstract
The invention discloses a method for processing sols of alumina refractory particles, which mainly aims to solve the problem of agglomeration of nano-powder during use in the prior art. The method comprises the following steps of: preparing magnalium precursor sols with a molar concentration of 0.5 to 2M from aluminium nitrate serving as an aluminum source, and magnesium oxalate or gnesium citrate serving as a magnesium source according to a mole ratio of Al to Mg of 2; putting the particles of aggregate particles of the alumina refractory material into an anti-acid container, and then pouring the magnalium precursor sols with a molar concentration of 0.5 to 2M into the container to soak for 5 to 10 minutes; after filtering the obtained objects by using a screen, putting the obtained particles into a sagger, and then carrying out thermal treatment on the obtained particles at the temperature of between 600 and 1,200 DEG C for 1 to 6 hours, and reacting the aluminosilicate refractory particles to synthesize nano magnesia-alumina spinel powder, and then obtain the aluminosilicate refractory particles attached with the nano magnesia-alumina spinel powder. The method of the invention has the advantage of uniformly-distributed nano-particles in the alumina refractory material can be used for processing refractory raw materials and improves the sintering process of the refractory raw materials.
Description
Technical field
The invention belongs to the material technology field, relate to the processing of aluminum fire resistant materials, a kind of especially method for processing sols of alumina refractory particles is adapted to the processing to the high alumina refractories particulate material.
Background technology
Nano material is little because of grain graininess, has bigger specific surface, thereby makes nano material show unusual small-size effect, specific surface effect and surfactivity free from worldly cares.In recent years, though people are means by experiment, as sol-gel method, vacuum freeze-drying methods etc. have prepared many refractory oxides, but nano particle is active significantly in actual applications, the agglomeration traits that shows, become the bottleneck of nano powder in refractory materials is used, restricted the application of nano material in refractory materials, the synthetic method of nano magnalium spinel is a lot, the research report of the aspect of relevant magnesium-aluminium spinel is quite a few both at home and abroad, but because the high reactivity of nano-grain, the agglomeration traits that produces in the nano powder use becomes the bottleneck problem that directly nano material is applied in the refractory materials.Add nano-oxide in the refractory materials research though also have, the actual report of using at refractory materials seldom to some extent.The research relevant with its research has following several:
Master's thesis " α-Al of the postgraduate Jia Xiaolin of University of Science ﹠ Technology, Beijing
2O
3The preparation of nano powder composite corundum brick, structure and performance study "; propose by the method for tensio-active agent; make nano particle have zeta-potential; to try hard to solve the agglomeration traits of nanometer; to obtain good effect modified by nano particles; but shortcoming is that nano powder is directly joined among the preparation technology of corundum brick, also be difficult to reach mix on technology, and the cost of nano-solid material is also bigger.
Li Xiaowei is at the paper " application of nanotechnology in unshape refractory " of " national unshape refractory proceeding in 2005 ", proposition is directly introduced presoma in the unshape refractory, realized the dispersive effect, but shortcoming is not relate to the technology that nanometer low temperature forms, the gas that the pyrolysis of presoma in use produces can make and occur pore in the material, reduces the use properties of material.
Zhang Haixia is at paper " the nanometer Al of " refractory materials "
2O
3To corundum based refractory materials structure and Effect on Performance " in; though propose to mix; this presoma viscosity is big; effect is not as other presoma with mechanical stirring and presoma aluminium colloidal sol and corundum in granules; and maximum shortcoming is to need whipping process; and also do not adopt the low temperature pretreatment technology, the gas of the pyrolysis of presoma generation makes the reduction of goods density equally.
People's such as Wang Houzhi patent ZL200510018955.0, a kind of method of magnesite refractory performance and product of producing with this method of improving proposed, but do not mention that technology and fire resisting material particle that nanometer low temperature forms coat problem, the material system that uses is a magnesite refractory, does not relate to the application of nano material in aluminum fire resistant materials.
Propose to utilize the spinel nano powder of sol-gel method preparation in the papers " Role of nanocrystalline spinel additive on the properties of lowcement castable refractories " of people in " Materials and Manufacturing Processes " such as India S.Mukhopadhyay, to the spinel pouring material add-on is 8.0wt.%, think that nano particle plays a part binding agent in matrix, this mould material shows good thermal shock resistance and slag resistance as middle ladle liner, does not also mention presoma low temperature and coats fire resisting material particle and subzero treatment technology.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, the method for processing sols of a kind of alumina refractory particles that provides to avoid the reunion of nano powder, is realized the even coating of nano powder to fire resisting material particle.
For achieving the above object, the present invention proposes following two kinds of technical schemes:
(1) nitrate and oxalate mixing precursor sol of preparation 0.5-2M volumetric molar concentration are put into this mixing precursor sol with alumina refractory particles and were flooded 5～10 minutes, take out behind screen filtration;
(2) particulate material behind the immersion filtration is placed in the saggar, places 600 ℃～1200 ℃ low temperature oven, be incubated 1～6 hour, make its magnalium presoma decompose the nano magnalium spinel powder that is evenly adhered on the surface of alumina refractory particles.
(1) nitrate and Citrate trianion mixing precursor sol of preparation 0.5-2M volumetric molar concentration are put into this mixing precursor sol with alumina refractory particles and were flooded 5～10 minutes, take out behind screen filtration;
(2) particulate material behind the immersion filtration is placed in the saggar, places 600 ℃～1200 ℃ low temperature oven, be incubated 1～6 hour, make its magnalium presoma decompose the nano magnalium spinel powder that is evenly adhered on the surface of alumina refractory particles.
Described colloidal sol is to be the aluminium source with the aluminum nitrate, is the magnesium source with magnesium citrate or magnesium oxalate, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is the magnalium precursor sol of 0.5～2M.
Described aluminum fire resistant materials comprises sintering magnesium-aluminium spinel, electric melting magnesium aluminum spinel, alundum and fused corundom.
The present invention has following advantage:
1. the present invention is owing to adopt the magnesium-aluminium spinel precursor solution to the alumina refractory particles dip treating, can realize the uniform mixing of molecular state, this wet chemical method is to the pretreatment of particles of raw materials of aluminium refractory material, can not only make nano particle uniform distribution in refractory raw material, solving the reunion bottleneck of nano particle, also is a kind of cheap practical application of nano powder in refractory materials;
2. the present invention is because with the low-temperature heat treatment of the particulate material behind the immersion filtration under 600 ℃～1200 ℃, the gas that can avoid aluminum fire resistant materials wherein pyrolytic reaction of presoma when high temperature uses to produce, in aluminum fire resistant materials, produce pore, the aluminum fire resistant materials performance is reduced;
3. the present invention helps promoting the sintering of aluminum fire resistant materials owing to the nano magnalium spinel powder that can evenly be adhered on the surface of alumina refractory particles.The raw materials of aluminium refractory material particle mostly is sintering magnesium-aluminium spinel, electric melting magnesium aluminum spinel, alundum and fused corundom, its chemically reactive is poor, sintering is difficulty very, therefore can make the nano magnalium spinel be coated on sintering magnesium-aluminium spinel, electric melting magnesium aluminum spinel, alundum and fused corundom particulate surface by the inventive method, make the nano magnalium spinel at high temperature play a part nanometer glue, with remarkable reduction sintering temperature.
Experiment shows: use present method can make the sintering temperature of aluminum fire resistant materials fall 100～200 ℃.
Description of drawings
The schema that the colloidal sol of Fig. 1 alumina refractory particles of the present invention is handled;
Fig. 2 is the alumina refractory particles diagrammatic cross-section after handling with the present invention.
Embodiment
With reference to Fig. 1, the present invention provides following six kinds of embodiment:
The first step, configuration presoma magnalium colloidal sol.
With the aluminum nitrate is the aluminium source, is the magnesium source with the magnesium citrate, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is nitrate and the Citrate trianion magnalium presoma mixed sols of 0.5M.
In second step, with alumina refractory particles, combined drive body colloidal sol flooded 5 minutes before for example sintering magnesium-aluminium spinel particle was put into nitrate and Citrate trianion magnalium, took out and sieved, and steeping fluid is separated with particulate material.This aluminum fire resistant materials adopts sintering magnesium-aluminium spinel or electric melting magnesium aluminum spinel or alundum or fused corundom.
The 3rd step, alumina refractory particles behind the dipping is carried out subzero treatment, particulate material after being about to sieve is positioned in the saggar through 600 ℃ of insulations 6 hours, reaction is synthetic on alumina refractory particles obtains the nano magnalium spinel powder, just can obtain being attached with the sintering magnesium-aluminium spinel particulate material of nano magnalium spinel powder.
The first step is the aluminium source with the aluminum nitrate, and magnesium citrate is the magnesium source, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is nitrate and the Citrate trianion magnalium presoma mixed sols of 2M.
In second step, with alumina refractory particles, for example the electric melting magnesium aluminum spinel particle is put into nitrate and Citrate trianion magnalium presoma mixed sols flooded 10 minutes, takes out and sieves, and steeping fluid is separated with particulate material.
The 3rd step, alumina refractory particles behind the dipping is carried out subzero treatment, particulate material after being about to sieve is positioned in the saggar through 1000 ℃ of insulations 3 hours, reaction is synthetic on alumina refractory particles obtains the nano magnalium spinel powder, just can obtain being attached with the electric melting magnesium aluminum spinel particulate material of nano magnalium spinel powder.
Embodiment 3, comprise the steps:
The first step is the aluminium source with the aluminum nitrate, is the magnesium source with the magnesium citrate, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is nitrate and the Citrate trianion magnalium presoma mixed sols of 1M.
In second step, with alumina refractory particles, for example the alundum particle is put into nitrate and Citrate trianion magnalium presoma mixed sols flooded 8 minutes, takes out and sieves, and steeping fluid is separated with particulate material.
The 3rd step, alundum particle behind the dipping is carried out subzero treatment, particulate material after being about to sieve is positioned in the saggar through 1200 ℃ of insulations 1 hour, reaction is synthetic on alumina refractory particles obtains the nano magnalium spinel powder, just can obtain being attached with the alundum particulate material of nano magnalium spinel powder.
Embodiment 4, comprise the steps:
The first step is the aluminium source with the aluminum nitrate, is the magnesium source with the magnesium oxalate, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is nitrate and the oxalate magnalium presoma mixed sols of 0.5M.
In second step, with alumina refractory particles, for example the fused corundom particle is put into nitrate and oxalate magnalium presoma mixed sols flooded 5 minutes, takes out and sieves, and steeping fluid is separated with particulate material.
The 3rd step, fused corundom particle behind the dipping is carried out subzero treatment, particulate material after being about to sieve is positioned in the saggar through 700 ℃ of insulations 5 hours, reaction is synthetic on alumina refractory particles obtains the nano magnalium spinel powder, just can obtain being attached with the fused corundom particulate material of nano magnalium spinel powder.
Embodiment 5, comprise the steps:
The first step is the aluminium source with the aluminum nitrate, is the magnesium source with the magnesium oxalate, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is nitrate and the oxalate magnalium presoma mixed sols of 2M.
In second step, with alumina refractory particles, for example sintering magnesium-aluminium spinel particle is put into nitrate and oxalate magnalium presoma mixed sols flooded 10 minutes, takes out and sieves, and steeping fluid is separated with particulate material.
The 3rd step, sintering magnesium-aluminium spinel particle behind the dipping is carried out subzero treatment, particulate material after being about to sieve is positioned in the saggar through 1000 ℃ of insulations 3 hours, reaction is synthetic on alumina refractory particles obtains the nano magnalium spinel powder, obtains being attached with the sintering magnesium-aluminium spinel particulate material of nano magnalium spinel powder.
Embodiment 6, comprise the steps:
The first step is the aluminium source with the aluminum nitrate, is the magnesium source with the magnesium oxalate, presses magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is nitrate and the oxalate magnalium presoma mixed sols of 1M.
In second step, with alumina refractory particles, for example the alundum particle is put into nitrate and oxalate magnalium presoma mixed sols flooded 8 minutes, takes out and sieves, and steeping fluid is separated with particulate material.
The 3rd step, alundum particle behind the dipping is carried out subzero treatment, particulate material after being about to sieve is positioned in the saggar through 1200 ℃ of insulations 1 hour, reaction is synthetic on alumina refractory particles obtains the nano magnalium spinel powder, just can obtain being attached with the alundum particulate material of nano magnalium spinel powder.
With the refractory materials after the inventive method processing as shown in Figure 2, wherein, 1 is alumina refractory particles, and 2 are reaction synthetic nano magnalium spinel powder.Experiment shows the preparation technology who the present invention is used for high alumina refractories can significantly reduce sintering temperature, has obtained good sintering as aluminium matter corundum refractory brick brick at 1500 ℃.
Claims (6)
1. the method for processing sols of an alumina refractory particles comprises the steps:
(1) nitrate and oxalate mixing presoma magnalium colloidal sol of preparation 0.5-2M volumetric molar concentration are put into this mixing precursor sol with alumina refractory particles and were flooded 5～10 minutes, take out behind screen filtration;
(2) particulate material behind the immersion filtration is placed in the saggar, places 600 ℃～1200 ℃ low temperature oven, be incubated 1～6 hour, make its magnalium presoma decompose the nano magnalium spinel powder that can evenly be adhered on the alumina refractory particles surface.
2. the method for processing sols of alumina refractory particles according to claim 1, wherein nitrate and oxalate mixing presoma magnalium colloidal sol are to be the aluminium source with the aluminum nitrate, are the magnesium source with the magnesium oxalate, press magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is the magnalium precursor sol of 0.5～2M.
3. the method for processing sols of alumina refractory particles according to claim 1, wherein said aluminum fire resistant materials comprises sintering magnesium-aluminium spinel, electric melting magnesium aluminum spinel, alundum and fused corundom.
4. the method for processing sols of an alumina refractory particles comprises the steps:
1) nitrate and Citrate trianion mixing presoma magnalium colloidal sol of preparation 0.5-2M volumetric molar concentration are put into this mixing precursor sol with alumina refractory particles and were flooded 5～10 minutes, take out behind screen filtration;
2) particulate material behind the immersion filtration is placed in the saggar, places 600 ℃～1200 ℃ low temperature oven, be incubated 1～6 hour, make its magnalium presoma decompose the nano magnalium spinel powder that can evenly be adhered on the alumina refractory particles surface.
5. the method for processing sols of alumina refractory particles according to claim 4, wherein nitrate and Citrate trianion mixing presoma magnalium colloidal sol are to be the aluminium source with the aluminum nitrate, are the magnesium source with the magnesium citrate, press magnesium-aluminium spinel MgAl
2O
4In aluminium and magnesium than the formula weight that is 2, preparing volumetric molar concentration is the magnalium precursor sol of 0.5～2M.
6. the method for processing sols of alumina refractory particles according to claim 4, wherein said aluminum fire resistant materials comprises sintering magnesium-aluminium spinel, electric melting magnesium aluminum spinel, alundum and fused corundom.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588052A (en) * | 2016-12-15 | 2017-04-26 | 河南瑞泰耐火材料科技有限公司 | Low-porosity chrome corundum brick and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215708A (en) * | 1997-10-27 | 1999-05-05 | 普拉塞尔技术有限公司 | Method for producing corrosion resistant refractories |
| CN101525247A (en) * | 2009-04-01 | 2009-09-09 | 郝富锁 | Method for processing aluminium refractory material by nanometer mullite |
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- 2010-07-16 CN CN 201010230998 patent/CN101913885A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215708A (en) * | 1997-10-27 | 1999-05-05 | 普拉塞尔技术有限公司 | Method for producing corrosion resistant refractories |
| CN101525247A (en) * | 2009-04-01 | 2009-09-09 | 郝富锁 | Method for processing aluminium refractory material by nanometer mullite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588052A (en) * | 2016-12-15 | 2017-04-26 | 河南瑞泰耐火材料科技有限公司 | Low-porosity chrome corundum brick and preparation method thereof |
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Application publication date: 20101215 |