CN109456069A - A kind of preparation method of densification Calcium dialuminate grog refractory - Google Patents
A kind of preparation method of densification Calcium dialuminate grog refractory Download PDFInfo
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
A kind of preparation method of densification Calcium dialuminate grog refractory, ingredient contain Al by weight percentage2O3 76.13 ~ 77.7%, CaO 20.87 ~ 21.3%, TiO2 1~3%；Relative density is 92.8 ~ 95.8%, and apparent porosity is 2.1 ~ 4.1%；The preparation method comprises the following steps: bauxite and lime stone are distinguished levigate rear mixing by (1)；(2) mixed material is pressed into green-ball, then carries out calcining for the first time and clinker is made；(3) by the levigate rear addition fine titanium dioxide powder of clinker, re-compacted balling-up；(4) second is carried out to calcine.The present invention is using fine titanium dioxide powder as rush agglutinant, it is dissolved into Calcium dialuminate phase in calcination process titanium dioxide and forms solid solution, to improve the sintering activity of Calcium dialuminate phase, promote growing up for Calcium dialuminate phase, so as to obtain fine and close Calcium dialuminate grog refractory under the conditions of lower secondary clacining temperature and shorter soaking time, production energy consumption is effectively reduced, production efficiency is improved, promotes energy-saving and emission-reduction.
Description
Technical field
The invention belongs to technical field of refractory materials, and in particular to a kind of preparation side of densification Calcium dialuminate grog refractory
Method.
Background technique
Calcium dialuminate (CA2) it is CaO-Al2O3Important high melting compound (1750 DEG C) in binary system have also
Stability is high in former, alkaline atmosphere, chemical resistance of concrete ability equal good characteristics by force, and its own thermal expansion coefficient is low, at the same with
Other high-melting-points, high-expansion material compound tense can be very good to reduce the thermal expansion coefficient of composite diphase material, have fairly good
Thermal shock resistance, therefore be it is extraordinary resistant to high temperatures, anti-erosion can be used for high temperature furnace lining, cylinder-packing etc., be high temperature insulating heat preservation
Novel refractory of good performance has good application prospect in the high temperature industry such as metallurgy, cement, glass, petrochemical industry.
On the other hand, aluminium oxide is widely used in fire resisting material field, due to the real density of aluminium oxide larger (4.10
g/cm3), cause the bulk density containing aluminum fire resistant materials larger, increases refractory material weight, do not only result in High-temp. kiln
Accumulation of heat loss increases, and also directly increases the discharge amount of used refractory.It is influenced simultaneously by bauxite resource problem, in recent years
Come, corundum cost of material persistently rises, and the production cost containing aluminum fire resistant materials is also high therewith；And lime stone is in the world
It is interior resourceful, and in CaO-Al2O3CA in binary system2With lesser real density (CA6, 3.79 g/cm3；CA2, 2.88
g/cm3), it is seen that as can producing CA with lime stone substitution part corundum2Fire proofed wood not only can be significantly reduced in lightweight refracrory
The production cost of material can also effectively realize the lightweight of refractory material, advantageously reduce high temperature furnace lining by reducing bulk density
Accumulation of heat with cylinder-packing is lost, and energy-saving and emission-reduction are promoted.
During synthesis in solid state prepares fine and close Calcium dialuminate grog refractory, by reacting adjoint between each constituent element
Volumetric expansion inhibits sintering and densification process, it is difficult to obtain fine and close grog refractory by once calcining；Meanwhile by
It is low in the sintering activity of Calcium dialuminate crystal phase, even if by calcining twice, it is also difficult to obtain fine and close clinker, general firing temperature is not
Lower than 1600 DEG C；Further, since easy dendrite interconnects to form porous structure between Calcium dialuminate crystal phase in reaction process, further influence
The sintering densification behavior of Calcium dialuminate refractory material.Densification Calcium dialuminate fire resisting disclosed in patent of invention CN105906355A
Clinker and preparation method thereof, principle are by adding Mn2+Replace Ca2+Form Ca(1-x)MnxAl4O7Two aluminium that solid solution improves
The sintering activity of sour calcium phase, the purpose of the promotion of the realization refractory material sintering densification.
Summary of the invention
For the above problem present on current Calcium dialuminate grog refractory technology of preparing, the present invention provides a kind of densifications
The preparation method of Calcium dialuminate grog refractory, principle are that addition fine titanium dioxide powder additive is laggard during rerolling
Row calcining, passes through Ti in calcination process4+Replace Al3+Form CaAl(4-4/3x)TixO7Solid solution, the burning of the Calcium dialuminate phase of raising
Knot activity, the Calcium dialuminate phase of promotion grows up, and can realize two under the conditions of lower calcination temperature and shorter soaking time
The good sintering of calcium aluminate grog refractory obtains fine and close Calcium dialuminate grog refractory, improves production efficiency, promotes energy-saving and emission-reduction.
Fine and close Calcium dialuminate grog refractory of the invention, ingredient contain Al by weight percentage2O3 76.13 ~ 77.7%, CaO
20.87 ~ 21.3%, TiO2 1~3%；Relative density is 92.8 ~ 95.8%, and apparent porosity is 2.1 ~ 4.1%.
The preparation method of fine and close Calcium dialuminate grog refractory of the invention, sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Close material；Wherein bauxite accounts for the 67.74% ~ 72.56% of mixed material total weight, and lime stone accounts for mixed material total weight
27.44%~32.26%；
(2) mixed material is pressed into green-ball under the pressure of 100 ~ 150MPa by ball press, by green-ball 1150 ~ 1200
1 ~ 2 hour is kept the temperature under the conditions of DEG C, first time calcining is carried out, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, addition fine titanium dioxide powder is simultaneously mixed in sand mixer,
Wherein fine titanium dioxide powder accounts for the 1 ~ 3% of clinker total weight；After mixing through ball press under the pressure of 100 ~ 150MPa
Balling-up is suppressed, secondary ball material is obtained；
(4) secondary ball material is kept the temperature 2 ~ 3 hours under the conditions of 1400 ~ 1450 DEG C, carries out second and calcines, obtain fine and close two aluminic acids
Calcium grog refractory.
Al in above-mentioned bauxite2O3Weight content >=75.6%, weight content >=50.6% of CaO in lime stone.
Above-mentioned fine titanium dioxide powder purity >=98%, granularity≤10 μm.
Compared with prior art, the features of the present invention and beneficial effect are:
The preparation method of fine and close Calcium dialuminate grog refractory of the invention, as agglutinant is promoted, is being calcined using fine titanium dioxide powder
Process passes through Ti4+Replace Al3+Form CaAl(4-4/3x)TixO7Solid solution makes Calcium dialuminate that distortion of lattice mutually occur, and activity improves,
It is promoted to be sintered and densification behavior, so as to be caused under the conditions of lower secondary clacining temperature and shorter soaking time
Close Calcium dialuminate grog refractory, effectively increases production efficiency, reduces production energy consumption and production cost.
Specific embodiment
The equipment that mixed material uses in the embodiment of the present invention is S1110 type sand mixer.
The equipment that compacting balling-up uses in the embodiment of the present invention is GY650-180 type ball press.
The equipment used is calcined in the embodiment of the present invention as high temperature vertical kiln.
Bauxite, lime stone and the fine titanium dioxide powder used in the embodiment of the present invention is commercial product.
Embodiment 1
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 75.6%, using the weight of CaO in lime stone
Measure percentage composition 54.8%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O3 77.7%, CaO 21.3%, TiO2
1%；Relative density is 92.8%, apparent porosity 4.1%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 72.56% of mixed material total weight, and lime stone accounts for the 27.44% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 150MPa by ball press, green-ball is protected under the conditions of 1200 DEG C
Temperature 2 hours carries out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, the fine titanium dioxide powder for accounting for clinker total weight 1% is added, mixed
After carrying out secondary mixing in sand machine, ball is pressed under the pressure of 150MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 2 hours under the conditions of 1450 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker；
In the case where not adding fine titanium dioxide powder, experiment is compared in a manner described, and the sintering for obtaining comparative experiments is ripe
Material；The sintered clinker of the fine and close Calcium dialuminate grog refractory of acquisition and comparative experiments is subjected to sem analysis respectively, the results showed that,
Sintered specimen interior tissue is loose under the conditions of additive-free, and stomata is more, in contrast, due to additive TiO2Addition, examination
The stomata of sample substantially reduces, and microstructure is obviously fine and close, can obviously observe its principal crystalline phase CA2Presence, from microstructure
Further illustrate additive TiO2Play the role of effectively promoting to the sintering of Calcium dialuminate；By two aluminic acid of densification of acquisition
Calcium grog refractory carries out EDS analysis, the results showed that, the TiO of addition2It is primarily present in inside system in Calcium dialuminate crystal phase,
Form CaAl(4-4/3x)TixO7Solid solution can promote Calcium dialuminate crystal phase that distortion of lattice occurs, and activity improves, and illustrate TiO2's
Sintering and the densification behavior for having effectively facilitated Calcium dialuminate is added.
Embodiment 2
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 77.7%, using the weight of CaO in lime stone
Measure percentage composition 54.3%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O377.54%, CaO 21.26%,
TiO21.2%；Relative density is 93.4%, apparent porosity 3.5%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 71.82% of mixed material total weight, and lime stone accounts for the 28.18% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 140MPa by ball press, green-ball is protected under the conditions of 1200 DEG C
Temperature 1 hour carries out first time calcining, a clinker is made；
(3) by a chamotte crushing and levigate to granularity≤88 mesh again, the titanium dioxide that addition accounts for clinker total weight 1.2% is micro-
Powder is mixed in sand mixer, is pressed into ball under the pressure of 150MPa by ball press, is obtained secondary ball material；
(4) secondary ball material is kept the temperature 3 hours under the conditions of 1450 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Embodiment 3
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 79.8%, using the weight of CaO in lime stone
Measure percentage composition 53.9%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O377.3%, CaO 21.2%, TiO2
1.5%；Relative density is 93.9%, apparent porosity 3.1%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 71.12% of mixed material total weight, and lime stone accounts for the 28.88% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 110MPa by ball press, green-ball is protected under the conditions of 1150 DEG C
Temperature 2 hours carries out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, addition accounts for the fine titanium dioxide powder of clinker total weight 1.5%,
It is mixed in sand mixer, ball is pressed under the pressure of 130MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 3 hours under the conditions of 1450 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Embodiment 4
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 80.9%, using the weight of CaO in lime stone
Measure percentage composition 53.3%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O3 77.07%, CaO 21.13%,
TiO2 1.8%；Relative density is 94.1%, apparent porosity 2.9%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 70.61% of mixed material total weight, and lime stone accounts for the 29.39% of mixed material total weight；
(2) mixed material is pressed into green-ball using ball press under the pressure of 100MPa by ball press, by green-ball 1150
1 hour is kept the temperature under the conditions of DEG C, first time calcining is carried out, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, addition accounts for the fine titanium dioxide powder of clinker total weight 1.8%,
It is mixed in sand mixer, ball is pressed under the pressure of 100MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 3 hours under the conditions of 1450 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Embodiment 5
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 82.5%, using the weight of CaO in lime stone
Measure percentage composition 52.8%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O3 76.91%, CaO 21.09%,
TiO22%；Relative density is 94.5%, apparent porosity 2.7%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 70.01% of mixed material total weight, and lime stone accounts for the 29.99% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 130MPa by ball press, green-ball is protected under the conditions of 1200 DEG C
Temperature 2 hours carries out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, the fine titanium dioxide powder for accounting for clinker total weight 2% is added, mixed
It is mixed in sand machine, ball is pressed under the pressure of 140MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 3 hours under the conditions of 1400 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Embodiment 6
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 84.9%, using the weight of CaO in lime stone
Measure percentage composition 51.9%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O376.52%, CaO 20.98%,
TiO2 2.5%；Relative density is 94.9%, apparent porosity 2.5%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 69.03% of mixed material total weight, and lime stone accounts for the 30.97% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 120MPa by ball press, green-ball is protected under the conditions of 1200 DEG C
Temperature 1 hour carries out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, addition accounts for the fine titanium dioxide powder of clinker total weight 2.5%,
It is mixed in sand mixer, ball is pressed under the pressure of 130MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 2 hours under the conditions of 1400 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Embodiment 7
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 86.6%, using the weight of CaO in lime stone
Measure percentage composition 51.3%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O376.28%, CaO 20.92%,
TiO22.8%；Relative density is 95.1%, apparent porosity 2.3%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 68.35% of mixed material total weight, and lime stone accounts for the 31.65% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 110MPa by ball press, green-ball is protected under the conditions of 1150 DEG C
Temperature 2 hours carries out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to grain≤88 mesh again, the fine titanium dioxide powder for accounting for clinker total weight 2.8% is added, mixed
It is mixed in sand machine, ball is pressed under the pressure of 120MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 2 hours under the conditions of 1400 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Embodiment 8
Al in the bauxite raw material used in the present embodiment2O3Weight percentage 87.9%, using the weight of CaO in lime stone
Measure percentage composition 50.6%.
The fine and close Calcium dialuminate grog refractory ingredient of preparation contains Al by weight percentage2O376.13%, CaO 20.87%,
TiO2 3%；Relative density is 95.8%, apparent porosity 2.1%；Preparation method sequentially includes the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Material is closed, wherein bauxite accounts for the 67.74% of mixed material total weight, and lime stone accounts for the 32.26% of mixed material total weight；
(2) mixed material is pressed into green-ball under the pressure of 100MPa by ball press, green-ball is protected under the conditions of 1150 DEG C
Temperature 1 hour carries out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, the fine titanium dioxide powder for accounting for clinker total weight 3% is added, mixed
It is mixed in sand machine, ball is pressed under the pressure of 110MPa by ball press, obtains secondary ball material；
(4) secondary ball material is kept the temperature 2 hours under the conditions of 1400 DEG C, carries out second and calcines, obtain fine and close Calcium dialuminate fire resisting
Clinker.
Claims (3)
1. a kind of preparation method of densification Calcium dialuminate grog refractory, it is characterised in that the densification Calcium dialuminate grog refractory at
It is grouped as by weight percentage as containing Al2O3 76.13 ~ 77.7%, CaO 20.87 ~ 21.3%, TiO2 1~3%；Product feature is phase
To density 92.8 ~ 95.8%, apparent porosity is 2.1 ~ 4.1%；Preparation method is characterized in that sequentially including the following steps:
(1) bauxite and lime stone is broken and levigate to granularity≤88 mesh respectively, after being mixed in sand mixer, it is made mixed
Close material；Wherein bauxite accounts for the 67.74% ~ 72.56% of mixed material total weight, and lime stone accounts for mixed material total weight
27.44%~32.26%；
(2) mixed material is pressed into green-ball under the pressure of 100 ~ 150MPa by ball press, by green-ball at 1150 ~ 1200 DEG C
Under the conditions of keep the temperature 1 ~ 2 hour, carry out first time calcining, clinker is made；
(3) by chamotte crushing and levigate to granularity≤88 mesh again, addition fine titanium dioxide powder is simultaneously mixed in sand mixer,
Wherein fine titanium dioxide powder accounts for the 1 ~ 3% of clinker total weight；The pressure by ball press in 100 ~ 150MPa pushes after mixing
Ball is made, obtains secondary ball material；
(4) secondary ball material is kept the temperature 2 ~ 3 hours under the conditions of 1400 ~ 1450 DEG C, carries out second and calcines, obtain fine and close two aluminic acids
Calcium grog refractory.
2. the preparation method of densification Calcium dialuminate grog refractory according to claim 1, it is characterised in that the dioxy
Change titanium micro mist purity >=98%, granularity≤10 μm.
3. the preparation method of densification Calcium dialuminate grog refractory according to claim 1, it is characterised in that the aluminium alum
Al in soil2O3Weight content >=75.6%, weight content >=50.6% of CaO in lime stone.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171980A (en) * | 2019-04-10 | 2019-08-27 | 辽宁科技学院 | A kind of preparation method of densification calcium hexaluminate grog refractory |
| CN113149670A (en) * | 2020-03-24 | 2021-07-23 | 辽宁科技学院 | Technological method for preparing compact calcium dialuminate refractory clinker by one-step method |
| CN113277839A (en) * | 2020-03-24 | 2021-08-20 | 辽宁科技学院 | One-step method for preparing compact CA2-CA6Technological process of complex phase refractory clinker |
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| US6689707B1 (en) * | 2003-04-01 | 2004-02-10 | Corning Incorporated | Low thermal expansion calcium aluminate articles |
| CN1714058A (en) * | 2002-12-19 | 2005-12-28 | 耐火材料控股有限公司 | Heavy ceramic moulded body, method for producing said body and use of the same |
| CN104692816A (en) * | 2015-02-10 | 2015-06-10 | 东北大学 | Compact aluminum, magnesium, calcium grog refractory and preparation method thereof |
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| CN1714058A (en) * | 2002-12-19 | 2005-12-28 | 耐火材料控股有限公司 | Heavy ceramic moulded body, method for producing said body and use of the same |
| US6689707B1 (en) * | 2003-04-01 | 2004-02-10 | Corning Incorporated | Low thermal expansion calcium aluminate articles |
| CN104692816A (en) * | 2015-02-10 | 2015-06-10 | 东北大学 | Compact aluminum, magnesium, calcium grog refractory and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110171980A (en) * | 2019-04-10 | 2019-08-27 | 辽宁科技学院 | A kind of preparation method of densification calcium hexaluminate grog refractory |
| CN113149670A (en) * | 2020-03-24 | 2021-07-23 | 辽宁科技学院 | Technological method for preparing compact calcium dialuminate refractory clinker by one-step method |
| CN113277839A (en) * | 2020-03-24 | 2021-08-20 | 辽宁科技学院 | One-step method for preparing compact CA2-CA6Technological process of complex phase refractory clinker |
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