CN105585314A - Dense calcium hexaluminate grog refractory and preparation method thereof - Google Patents
Dense calcium hexaluminate grog refractory and preparation method thereof Download PDFInfo
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- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
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- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- 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
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/604—Pressing at temperatures other than sintering temperatures
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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Abstract
The invention discloses a dense calcium hexaluminate grog refractory and a preparation method thereof. The refractory is prepared from, by weight, 87.04-88.87% of Al2O3, 7.96-8.13% of CaO and 3.00-5.00% of MnO, wherein the relative density is 90.90-94.80%, and the apparent porosity is 2.80-4.40%. The preparation method includes the steps of firstly, grinding and mixing bauxite and limestone; secondly, pressing the mixture into raw balls, and primarily calcining the raw balls to prepare clinker; thirdly, adding manganous oxide fine powder after clinker is ground fine, and pressing the mixture into balls; fourthly, conducting secondary calcining. The manganous oxide fine powder is adopted as a sintering promoter, solid manganous oxide is dissolved in a calcium hexaluminate phase in the calcining process to form a solid solution, and therefore the sintering activity of the calcium hexaluminate phase is improved, the growth of the calcium hexaluminate phase is promoted, and therefore the dense calcium hexaluminate grog refractory can be obtained at a low secondary calcining temperature within a short heat preservation time, production energy consumption is effectively lowered, production efficiency is improved, and energy conservation and emission reduction are promoted.
Description
Technical field
The invention belongs to technical field of refractory materials, be specifically related to a kind of fine and close calcium hexaluminate grog refractory and preparation method thereof.
Background technology
Calcium hexaluminate (CA6) fusing point high (1870 DEG C), fire resistance is good, solubility in iron content slag is low, stability in reducing atmosphere (CO) is high, chemical stability in alkaline environment is good, wetability to motlten metal and slag (iron and steel and non-ferrous metal) is low, therefore be extraordinary high temperature resistance, anti-erosion, anti-molten metal and slag infiltrate, there is high temperature insulating heat-insulating property material, and can be directly used in the novel refractory that metallurgical furnace lining contacts with molten metal and fused salt with metallurgical cylinder-packing hot side. Simultaneously, calcium hexaluminate and aluminium oxide have good chemical compatibility and close thermal expansivity, can be used in conjunction with any ratio with aluminium oxide, these characteristics make calcium hexaluminate have application prospect very widely in high temperature industries such as metallurgy, glass, cement, pottery, petrochemical industries.
In the process of the fine and close calcium hexaluminate grog refractory of the synthetic preparation of solid phase, because the Volumetric expansion that reacts followed between each constituent element has suppressed sintering and densification process, be difficult to obtain fine and close grog refractory by once calcining; Meanwhile, because the sintering activity of calcium hexaluminate phase is low, even by twice calcining, be also difficult to obtain fine and close grog, therefore General Requirements firing temperature is not less than 1700 DEG C; In addition,, due to the easy dendrite mesh structural porous structure of interconnected formation of putting up a bridge between calcium hexaluminate crystalline phase in course of reaction, further affected the sintering densification of calcium hexaluminate refractory material.
Summary of the invention
For the problems referred to above that exist in current calcium hexaluminate grog refractory technology of preparing, the invention provides a kind of fine and close calcium hexaluminate grog refractory and preparation method thereof, to calcine by add manganese monoxide micro-powder as additive in rerolling process after, by be solidly soluted at calcination process manganese monoxide calcium hexaluminate quite in, thereby form the sintering activity of solid solution raising calcium hexaluminate phase, promote growing up of calcium hexaluminate phase, can under lower calcining heat and shorter temperature retention time condition, realize the good sintering of calcium hexaluminate grog refractory, obtain fine and close calcium hexaluminate grog refractory, enhance productivity, promote energy-saving and emission-reduction.
Fine and close calcium hexaluminate grog refractory of the present invention, its composition is by weight percentage containing Al2O387.04 ~ 88.87%, CaO7.96 ~ 8.13%, MnO3.00 ~ 5.00%; Relative density is 90.90 ~ 94.80%, and apparent porosity is 2.80 ~ 4.40%.
The preparation method of fine and close calcium hexaluminate grog refractory of the present invention, carries out according to the following steps:
(1) by broken and levigate to granularity≤88 order respectively to bauxite and lime stone, after mixing, make mixed material in puddle mixer; Wherein bauxite accounts for 86.38% ~ 88.90% of mixed material gross weight, and lime stone accounts for 11.10% ~ 13.62% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 100 ~ 150MPa, green-ball is incubated to 1 ~ 2 hour under 1200 ~ 1250 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add manganese monoxide micro mist and mix in puddle mixer, wherein manganese monoxide micro mist accounts for 3.00 ~ 5.00% of grog gross weight; After mixing, under the pressure of 100 ~ 150MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 2 ~ 3 hours under 1600 ~ 1650 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Al in above-mentioned bauxite2O3Weight content >=74.20%, weight content >=50.20% of CaO in lime stone.
Above-mentioned manganese monoxide micro mist purity >=98.00%, granularity≤10 μ m.
Compared with prior art, feature of the present invention and beneficial effect are:
Fine and close calcium hexaluminate grog refractory of the present invention adopts manganese monoxide micro mist as short agglutinant, calcination process manganese monoxide be solidly soluted into calcium hexaluminate mutually in, make calcium hexaluminate that distortion of lattice occur mutually, active raising, promote its sintering and densification behavior, thereby can under lower secondary clacining temperature and shorter temperature retention time condition, obtain fine and close calcium hexaluminate grog refractory, effectively improve production efficiency, reduce energy consumption and production cost.
Detailed description of the invention
The equipment that in the embodiment of the present invention, mixed material adopts is S1110 type puddle mixer.
The equipment of suppressing balling-up employing in the embodiment of the present invention is GY650-180 type ball press.
The equipment that in the embodiment of the present invention, calcining adopts is high temperature vertical kiln.
The bauxite, magnesite, lime stone and the manganese monoxide micro mist that in the embodiment of the present invention, adopt are commercially available prod.
Embodiment 1
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 74.20%, adopt the weight percentage 54.50% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O388.87%, CaO8.13%, MnO3.00%; Relative density is 90.90%, and apparent porosity is 4.40%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 88.90% of mixed material gross weight, and lime stone accounts for 11.10% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 150MPa, green-ball is incubated to 2 hours under 1250 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 3.00%, in puddle mixer, carry out, after secondary mixing, under the pressure of 150MPa, being pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 3 hours under 1650 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory;
In the situation that not adding manganese monoxide micro mist, carry out in a manner described contrast experiment, obtain contrast experiment's sintered clinker; The fine and close calcium hexaluminate grog refractory obtaining and contrast experiment's sintered clinker are carried out respectively to sem analysis, result shows, under additive-free condition, sintered specimen interior tissue is loose, pore is more, by contrast, due to adding of additive MnO, the pore of sample significantly reduces, microstructure is obviously fine and close, can clearly observe its principal crystalline phase CA6Existence, further illustrate additive MnO from microstructure the sintering of calcium hexaluminate refractory material played to effective facilitation; The fine and close calcium hexaluminate grog refractory obtaining is carried out to EDS analysis, result shows, the MnO adding is mainly present in the middle of the inner calcium hexaluminate crystalline phase of system, form solid solution, can impel calcium hexaluminate crystalline phase generation distortion of lattice, active raising, illustrates adding of MnO of effective sintering and densification behavior that has promoted calcium hexaluminate.
Embodiment 2
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 75.60%, adopt the weight percentage 54.00% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O388.60%, CaO8.10%, MnO3.30%; Relative density is 91.70%, and apparent porosity is 4.20%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 88.62% of mixed material gross weight, and lime stone accounts for 11.38% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 140MPa, green-ball is incubated to 2 hours under 1250 DEG C of conditions, calcine for the first time, make grog one time;
(3) by a chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 3.30%, in puddle mixer, mix, under the pressure of 150MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 2 hours under 1650 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Embodiment 3
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 77.80%, adopt the weight percentage 53.80% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O388.41%, CaO8.09%, MnO3.50%; Relative density is 92.40%, and apparent porosity is 3.90%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 88.29% of mixed material gross weight, and lime stone accounts for 11.71% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 120MPa, green-ball is incubated to 2 hours under 1200 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 3.50%, in puddle mixer, mix, under the pressure of 140MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 3 hours under 1650 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Embodiment 4
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 79.70%, adopt the weight percentage 53.20% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O388.14%, CaO8.06%, MnO3.80%; Relative density is 93.30%, and apparent porosity is 3.60%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 87.92% of mixed material gross weight, and lime stone accounts for 12.08% of mixed material gross weight;
(2) under the pressure of 100MPa, adopt ball press to be pressed into green-ball by ball press mixed material, green-ball is incubated to 1 hour under 1200 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 3.80%, in puddle mixer, mix, under the pressure of 100MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 3 hours under 1650 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Embodiment 5
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 80.50%, adopt the weight percentage 52.60% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O387.96%, CaO8.04%, MnO4.00%; Relative density is 93.70%, and apparent porosity is 3.40%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 87.57% of mixed material gross weight, and lime stone accounts for 12.43% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 130MPa, green-ball is incubated to 2 hours under 1250 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 4.00%, in puddle mixer, mix, under the pressure of 150MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 3 hours under 1600 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Embodiment 6
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 82.10%, adopt the weight percentage 51.90% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O387.59%, CaO8.01%, MnO4.40%; Relative density is 94.10%, and apparent porosity is 3.10%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 87.33% of mixed material gross weight, and lime stone accounts for 12.67% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 120MPa, green-ball is incubated to 2 hours under 1250 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 4.40%, in puddle mixer, mix, under the pressure of 130MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 2 hours under 1600 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Embodiment 7
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 84.70%, adopt the weight percentage 51.10% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O387.31%, CaO7.99%, MnO4.70%; Relative density is 94.50%, and apparent porosity is 3.00%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 86.81% of mixed material gross weight, and lime stone accounts for 13.19% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 110MPa, green-ball is incubated to 1 hour under 1200 DEG C of conditions, calcine for the first time, make grog;
(3) add to grain≤88 orders the manganese monoxide micro mist that accounts for grog gross weight 4.70% by also again levigate chamotte crushing, in puddle mixer, mix, under the pressure of 120MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 2 hours under 1600 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Embodiment 8
Al in the bauxite raw material adopting in the present embodiment2O3Weight percentage 86.30%, adopt the weight percentage 50.20% of CaO in lime stone.
The fine and close calcium hexaluminate grog refractory composition of preparation is by weight percentage containing Al2O387.04%, CaO7.96%, MnO5.00%; Relative density is 94.80%, and apparent porosity is 2.80%; Preparation method carries out according to the following steps:
(1) bauxite, magnesite and lime stone is broken and levigate to granularity≤88 order respectively, after mixing, make mixed material in puddle mixer, wherein bauxite accounts for 86.38% of mixed material gross weight, and lime stone accounts for 13.62% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 100MPa, green-ball is incubated to 1 hour under 1200 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add the manganese monoxide micro mist that accounts for grog gross weight 5.00%, in puddle mixer, mix, under the pressure of 110MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 2 hours under 1600 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
Claims (4)
1. a fine and close calcium hexaluminate grog refractory, is characterized in that composition is by weight percentage containing Al2O387.04 ~ 88.87%, CaO7.96 ~ 8.13%, MnO3.00 ~ 5.00%; Relative density is 90.90 ~ 94.80%, and apparent porosity is 2.80 ~ 4.40%.
2. a preparation method for fine and close calcium hexaluminate grog refractory claimed in claim 1, is characterized in that carrying out according to the following steps:
(1) by broken and levigate to granularity≤88 order respectively to bauxite and lime stone, after mixing, make mixed material in puddle mixer; Wherein bauxite accounts for 86.38% ~ 88.90% of mixed material gross weight, and lime stone accounts for 11.10% ~ 13.62% of mixed material gross weight;
(2) mixed material is pressed into green-ball by ball press under the pressure of 100 ~ 150MPa, green-ball is incubated to 1 ~ 2 hour under 1200 ~ 1250 DEG C of conditions, calcine for the first time, make grog;
(3) by chamotte crushing again levigate to granularity≤88 order, add manganese monoxide micro mist and mix in puddle mixer, wherein manganese monoxide micro mist accounts for 3.00 ~ 5.00% of grog gross weight; After mixing, under the pressure of 100 ~ 150MPa, be pressed into ball by ball press, obtain secondary ball material;
(4) secondary ball material is incubated to 2 ~ 3 hours under 1600 ~ 1650 DEG C of conditions, calcines for the second time, obtain fine and close calcium hexaluminate grog refractory.
3. the preparation method of fine and close calcium hexaluminate grog refractory according to claim 2, is characterized in that described manganese monoxide micro mist purity >=98.00%, granularity≤10 μ m.
4. the preparation method of fine and close calcium hexaluminate grog refractory according to claim 2, is characterized in that Al in described bauxite2O3Weight content >=74.20%, weight content >=50.20% of CaO in lime stone.
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WO2022237776A1 (en) | 2021-05-10 | 2022-11-17 | 淄博郎丰高温材料有限公司 | Ca6-based refractory material with medium volume density, preparation method therefor, and use thereof |
WO2022237717A1 (en) | 2021-05-10 | 2022-11-17 | 淄博市鲁中耐火材料有限公司 | High-purity compact calcium hexa-aluminate-based refractory material and preparation method therefor |
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