CN111099891A - Technological method for preparing compact calcium hexaluminate refractory clinker by one-step method - Google Patents

Technological method for preparing compact calcium hexaluminate refractory clinker by one-step method Download PDF

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Publication number
CN111099891A
CN111099891A CN202010033423.9A CN202010033423A CN111099891A CN 111099891 A CN111099891 A CN 111099891A CN 202010033423 A CN202010033423 A CN 202010033423A CN 111099891 A CN111099891 A CN 111099891A
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calcium hexaluminate
mixed material
limestone
micro powder
bauxite
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尹雪亮
马贺利
杜成武
宫长伟
李丽颖
彭可武
韩廷全
丁洪海
尹雪冬
张博
段磊
郭少卿
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Liaoning Institute of Science and Technology
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Liaoning Institute of Science and Technology
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Priority to CN202010033423.9A priority Critical patent/CN111099891A/en
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Priority to CN202110033908.2A priority patent/CN112707725A/en
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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
    • C04B35/44—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 aluminates
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • 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
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • 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
    • C04B2235/3205—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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

A one-step process for preparing compact calcium hexaluminate refractory clinker contains Al2O387.96-89.79%, CaO 8.04-8.21%, and A micropowder 2.00-4.00%; the relative density is 91.30-94.60%, and the apparent porosity is 2.80-4.50%; the preparation method comprises the following steps: (1) respectively grinding bauxite, limestone and A micro powder and then mixing; (2) pressing the mixed material into green pellets, and calcining to obtain clinker. The invention adopts the A micro powder as the sintering promoting agent, and the A micro powder is dissolved in the calcium hexaluminate phase to form a solid solution in the calcining process, thereby improving the sintering activity of the calcium hexaluminate phase, promoting the growth of the calcium hexaluminate phase, obtaining the compact calcium hexaluminate refractory clinker under the conditions of lower calcining temperature and shorter heat preservation time, effectively reducing the production energy consumption, improving the production efficiency,promoting energy conservation and emission reduction.

Description

Technological method for preparing compact calcium hexaluminate refractory clinker by one-step method
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a process method for preparing compact calcium hexaluminate refractory clinker by a one-step method.
Background
Calcium hexaluminate (CA)6) The material has the advantages of high melting point (1870 ℃), good fire resistance, low solubility in iron-containing slag, high stability in reducing atmosphere (CO), good chemical stability in alkaline environment and low wettability to molten metal and slag (steel and nonferrous metal), so the material is a novel refractory material which has good high temperature resistance, erosion resistance and molten slag infiltration resistance, has high-temperature heat insulation performance, and can be directly used for metallurgical furnace linings and metallurgical ladle lining hot surfaces, and the contact of molten metal and molten salt. Meanwhile, the calcium hexaluminate has good chemical compatibility and similar thermal expansion property with alumina, and can be matched with the alumina in any proportion, and the characteristics ensure that the calcium hexaluminate has very wide application prospect in high-temperature industries such as metallurgy, glass, cement, ceramics, petrochemical industry and the like.
In the process of preparing the compact calcium hexaluminate refractory clinker by solid phase synthesis, the volume expansion effect accompanied by the reaction among the components of each raw material inhibits the sintering and densification processes, meanwhile, the sintering activity of the calcium hexaluminate phase is low, the compact clinker is difficult to obtain even through high-temperature calcination, and in addition, the sintering densification of the calcium hexaluminate refractory material is further influenced because the calcium hexaluminate crystal phases are easy to form a network porous structure by dendritic bridging and interconnection in the reaction process. The invention discloses a preparation method of compact calcium hexaluminate refractory clinker disclosed in patent CN105585314B and patent CN110171980A, the technological process is a production mode of adopting a two-step method, namely, one-step presintering to eliminate volume expansion effect, and two-step sintering to densify, and the technological process is complex, the energy consumption is large, and the production cost is high.
Disclosure of Invention
Aiming at the problems in the existing preparation technology of the calcium hexaluminate refractory clinker, the invention provides a one-step process for preparing the compact calcium hexaluminate refractory clinker, which is based on the principle that a micropowder additive A is added in the material mixing process and then calcined, the micropowder A is dissolved in a calcium hexaluminate crystal phase in the calcining process to form a solid solution, so that the sintering activity of the calcium hexaluminate phase is enhanced powerfully, the growth of the calcium hexaluminate phase is promoted effectively, the good sintering of the calcium hexaluminate refractory clinker can be realized under the conditions of lower calcining temperature and shorter heat preservation time by a one-step method, the compact calcium hexaluminate refractory clinker is obtained, the production efficiency is improved, and the energy conservation and emission reduction are promoted.
The compact calcium hexaluminate refractory clinker comprises Al in percentage by weight2O387.96-89.79%, CaO 8.04-8.21%, and A micropowder 2.00-4.00%; the relative density is 91.30-94.60%, and the apparent porosity is 2.80-4.50%.
The preparation method of the compact calcium hexaluminate refractory clinker comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone until the granularity is less than or equal to 88 meshes, adding A micro powder, and mixing in a sand mixer to prepare a mixed material; wherein the bauxite accounts for 83.61-87.37% of the total weight of the mixed material, the limestone accounts for 11.15-13.12% of the total weight of the mixed material, and the A micro powder accounts for 1.5-3.3% of the total weight of the mixed material;
(2) pressing the mixed material into green balls by a ball press machine under the pressure of 120-150 MPa;
(3) and (3) keeping the temperature of the green pellets at 1600-1650 ℃ for 2-2.5 hours, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Al in the above-mentioned bauxite2O3The weight content of the limestone is more than or equal to 76.20 percent, and the weight content of CaO in the limestone is more than or equal to 50.20 percent.
The purity of the A micro powder is more than or equal to 98.00 percent, and the granularity is less than or equal to 10 mu m.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
the compact calcium hexaluminate refractory clinker adopts the A micro powder as a sintering promoting agent, and the A micro powder is dissolved in the calcium hexaluminate phase in a solid solution manner in the calcining process, so that the calcium hexaluminate phase generates lattice distortion, the activity is greatly improved, and the sintering and densification behaviors are promoted, so that the compact calcium hexaluminate refractory clinker can be obtained by a one-step method under the conditions of lower calcining temperature and shorter heat preservation time, the production efficiency is greatly improved, and the production energy consumption and the production cost are reduced.
Detailed Description
The equipment adopted for mixing the materials in the embodiment of the invention is an S1110 type sand mixer.
The equipment used for pressing the balls in the embodiment of the invention is a GY650-180 type ball press machine.
The equipment adopted for calcination in the embodiment of the invention is a high-temperature shaft kiln.
Bauxite, limestone and A micro powder adopted in the embodiment of the invention are commercial products.
Example 1
Al in the raw bauxite employed in this example2O376.20 percent by weight, and 54.60 percent by weight of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O389.79 percent, CaO 8.21 percent and A micro powder 2.00 percent; the relative density is 91.30%, and the apparent porosity is 4.50%; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, adding A micro powder, and mixing in a sand mixer to prepare a mixed material, wherein the bauxite accounts for 87.37% of the total weight of the mixed material, the limestone accounts for 11.15% of the total weight of the mixed material, and the A micro powder accounts for 1.48% of the total weight of the mixed material;
(2) and pressing the mixed materials into green balls by a ball press machine under the pressure of 150MPa, preserving the heat of the green balls for 2.5 hours at 1650 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Under the condition of not adding the A micro powder, carrying out a comparison experiment according to the mode to obtain sintered clinker of the comparison experiment; SEM analysis is respectively carried out on the obtained compact calcium hexaluminate refractory clinker and the sintered clinker in the comparative experiment, and the result shows that the internal structure of the sintered sample is loose and has more air holes under the condition of no additive, in contrast, the air holes of the sample are obviously reduced and the microstructure is obviously compact due to the addition of the additive A, and the main crystal phase CA of the compact calcium hexaluminate refractory clinker can be clearly observed6The existence of the additive A is further proved from the microstructure that the additive A has an effective promoting effect on the sintering of the calcium hexaluminate refractory material; EDS analysis is carried out on the obtained compact calcium hexaluminate refractory clinker, and the result shows that the added A mainly exists in a calcium hexaluminate crystal phase in a system to form a solid solution, so that the crystal lattice distortion of the calcium hexaluminate crystal phase is promoted, the activity is improved, and the sintering and densification behaviors of the calcium hexaluminate are effectively promoted by adding the additive A.
Example 2
Al in the raw bauxite employed in this example2O377.50 wt%, and 53.70 wt% of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O389.60 percent, CaO 8.20 percent and A micro powder 2.20 percent; the relative density is 91.90%, and the apparent porosity is 4.30%; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, adding A micro powder, and mixing in a sand mixer to prepare a mixed material, wherein the bauxite accounts for 86.88% of the total weight of the mixed material, the limestone accounts for 11.47% of the total weight of the mixed material, and the A micro powder accounts for 1.65% of the total weight of the mixed material;
(2) and pressing the mixed material into green balls by a ball press machine under the pressure of 140MPa, preserving the heat of the green balls for 2.5 hours at 1650 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Example 3
Al in the raw bauxite employed in this example2O378.80 wt%, and 53.10 wt% of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O389.33%, CaO 8.17%, A micropowder 2.50%; the relative density is 92.50 percent, and the apparent porosity is 3.90 percent; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, adding A micro powder, and mixing in a sand mixer to prepare a mixed material, wherein the bauxite accounts for 86.37 percent of the total weight of the mixed material, the limestone accounts for 11.72 percent of the total weight of the mixed material, and the A micro powder accounts for 1.9 percent of the total weight of the mixed material;
(2) and pressing the mixed material into green balls by a ball press machine under the pressure of 130MPa, preserving the temperature of the green balls for 2 hours at 1650 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Example 4
Al in the raw bauxite employed in this example2O379.40 wt%, and the weight percentage of CaO in the limestone is 52.70 wt%.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O389.05 percent, CaO 8.15 percent and A micro powder 2.80 percent; the relative density is 93.20%, and the apparent porosity is 3.60%; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, adding A micro powder, and mixing in a sand mixer to prepare a mixed material, wherein the bauxite accounts for 86.00% of the total weight of the mixed material, the limestone accounts for 11.85% of the total weight of the mixed material, and the A micro powder accounts for 2.15% of the total weight of the mixed material;
(2) and pressing the mixed materials into green balls by a ball press machine under the pressure of 120MPa, preserving the heat of the green balls for 2 hours at 1650 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Example 5
Al in the raw bauxite employed in this example2O380.30 percent by weight, and 52.10 percent by weight of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O388.87%, CaO 8.13%, A micropowder 3.00%; the relative density is 93.70 percent, and the apparent porosity is 3.40 percent; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, and mixing the bauxite and the limestone in a sand mixer after adding A micro powder to prepare a mixed material, wherein the bauxite accounts for 85.61 percent of the total weight of the mixed material, the limestone accounts for 12.07 percent of the total weight of the mixed material, and the A micro powder accounts for 2.32 percent of the total weight of the mixed material;
(2) pressing the mixed materials into green balls by a ball press machine under the pressure of 150MPa, preserving the temperature of the green balls for 2.5 hours at the temperature of 1600 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Example 6
Al in the raw bauxite employed in this example2O382.20 wt%, and 51.80 wt% of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O388.69%, CaO 8.11%, A micropowder 3.20%; the relative density is 94.10%, and the apparent porosity is 3.20%; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, and mixing the bauxite and the limestone in a sand mixer after adding A micro powder to prepare a mixed material, wherein the bauxite accounts for 85.12 percent of the total weight of the mixed material, the limestone accounts for 12.35 percent of the total weight of the mixed material, and the A micro powder accounts for 2.52 percent of the total weight of the mixed material;
(2) and pressing the mixed materials into green balls by a ball press machine under the pressure of 140MPa, preserving the temperature of the green balls for 2.5 hours at 1600 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Example 7
Al in the raw bauxite employed in this example2O384.30 percent by weight, and 51.30 percent by weight of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O388.41%, CaO 8.09%, and A micropowder 3.50%; the relative density is 94.40%, and the apparent porosity is 3.00%; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, and mixing the bauxite and the limestone in a sand mixer after adding A micro powder to prepare a mixed material, wherein the bauxite accounts for 84.48% of the total weight of the mixed material, the limestone accounts for 12.70% of the total weight of the mixed material, and the A micro powder accounts for 2.82% of the total weight of the mixed material;
(2) pressing the mixed materials into green balls by a ball press machine under the pressure of 130MPa, preserving the temperature of the green balls for 2 hours at 1600 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.
Example 8
Al in the raw bauxite employed in this example2O386.10% by weight, and 50.20% by weight of CaO in the limestone.
The prepared compact calcium hexaluminate refractory clinker component contains Al according to weight percentage2O387.96%, CaO 8.04%, A micropowder 4.00%; the relative density is 94.60 percent, and the apparent porosity is 2.80 percent; the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone to a particle size of less than or equal to 88 meshes, and mixing the bauxite and the limestone in a sand mixer after adding A micro powder to prepare a mixed material, wherein the bauxite accounts for 83.61% of the total weight of the mixed material, the limestone accounts for 13.12% of the total weight of the mixed material, and the A micro powder accounts for 3.27% of the total weight of the mixed material;
(2) pressing the mixed materials into green balls by a ball press machine under the pressure of 120MPa, preserving the temperature of the green balls for 2 hours at 1600 ℃, and calcining to obtain the compact calcium hexaluminate refractory clinker.

Claims (3)

1. A one-step process for preparing compact calcium hexaluminate refractory clinker is characterized in that the components contain Al according to weight percentage2O387.96-89.79%, CaO 8.04-8.21%, and A micropowder 2.00-4.00%; the relative density is 91.30-94.60%, the apparent porosity is 2.80-4.50%, and the preparation method comprises the following steps:
(1) respectively crushing and grinding bauxite and limestone until the granularity is less than or equal to 88 meshes, adding A micro powder, and mixing in a sand mixer to prepare a mixed material; wherein the bauxite accounts for 83.61-87.37% of the total weight of the mixed material, the limestone accounts for 11.15-13.12% of the total weight of the mixed material, and the A micro powder accounts for 1.5-3.3% of the total weight of the mixed material;
(2) pressing the mixed material into green balls by a ball press machine under the pressure of 120-150 MPa;
(3) and (3) keeping the temperature of the green pellets at 1600-1650 ℃ for 2-2.5 hours, and calcining to obtain the compact calcium hexaluminate refractory clinker.
2. The dense calcium hexaluminate refractory clinker of claim 1, wherein the purity of the micropowder A is not less than 98.00%, and the particle size is not more than 10 μm.
3. The dense calcium hexaluminate refractory clinker of claim 1, wherein Al is in bauxite2O3The weight content of the limestone is more than or equal to 76.20 percent, and the weight content of CaO in the limestone is more than or equal to 50.20 percent.
CN202010033423.9A 2020-01-13 2020-01-13 Technological method for preparing compact calcium hexaluminate refractory clinker by one-step method Pending CN111099891A (en)

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CN111099891A (en) * 2020-01-13 2020-05-05 辽宁科技学院 Technological method for preparing compact calcium hexaluminate refractory clinker by one-step method
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CN108439961A (en) * 2018-05-21 2018-08-24 中钢集团洛阳耐火材料研究院有限公司 A kind of preparation method of the high-purity calcium hexaluminate of densification-corundum composite diphase material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112707725A (en) * 2020-01-13 2021-04-27 辽宁科技学院 Technological method for preparing compact calcium hexaluminate refractory clinker by one-step method

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