CN111205099A - Batch-type operation high-temperature kiln near-zero heat loss refractory material lining body and preparation method thereof - Google Patents

Batch-type operation high-temperature kiln near-zero heat loss refractory material lining body and preparation method thereof Download PDF

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CN111205099A
CN111205099A CN202010065422.2A CN202010065422A CN111205099A CN 111205099 A CN111205099 A CN 111205099A CN 202010065422 A CN202010065422 A CN 202010065422A CN 111205099 A CN111205099 A CN 111205099A
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silicon
aluminum
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alloy
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CN111205099B (en
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张美杰
顾华志
王瑶
黄奥
付绿平
杨爽
夏求林
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
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    • 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
    • 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
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/404—Refractory metals
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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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon

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Abstract

The invention relates to a near-zero heat loss refractory material lining body of an intermittently operated high-temperature kiln and a preparation method thereof, and the technical scheme is that a permanent lining refractory material of the refractory material lining body is a phase change heat storage refractory material, namely a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material are sequentially composed from inside to outside, wherein the phase change heat storage refractory material is composed of an alloy @ ceramic large capsule, an alloy @ alumina microcapsule, α -Al2O3Mixing the micro powder, the silicon micro powder, the calcium aluminate cement and the polycarboxylic acid with water, and carrying out molding, demolding and drying to obtain the calcium aluminate cement. During preparation: aluminum-silicon-nickel alloy @ ceramic macrocapsules, aluminum-silicon-iron alloy @ ceramic macrocapsules and aluminum-silicon alloy @ ceramic macrocapsules of the alloy @ ceramic macrocapsules are respectively prepared from corresponding aluminum-silicon-nickel alloy @ alumina microcapsules, aluminum-silicon-iron alloy @ alumina microcapsules and aluminum-silicon alloy @ alumina microcapsules in the aluminum-silicon alloy @ ceramic macrocapsules and the alloy @ alumina microcapsules. Hair brushThe apparent heat loss is approximately zero and the service life of the refractory material of the furnace lining is long.

Description

Batch-type operation high-temperature kiln near-zero heat loss refractory material lining body and preparation method thereof
Technical Field
The invention belongs to the technical field of batch operation high-temperature kiln liners. In particular to a near-zero heat loss refractory material lining body for intermittently operating a high-temperature kiln and a preparation method thereof.
Background
The energy is the basis of social development, the industrial energy consumption accounts for 32-35% of the global total energy consumption, and the national industrial energy consumption is as high as 70% of the total energy consumption. High temperature industrial furnaces are the major energy consumers, accounting for more than 48% of industrial energy consumption (Laveet Kumar, M.Hasanuzaman, N.A.Rahim.Global advance of solar thermal energy technologies for industrial process heat and its future processes, Areve. energy Conversion and Management,2019,195:885 + 908). The furnace lining refractory material has decisive influence on the energy consumption of the industrial furnace, and generally, according to heat transfer calculation, a plurality of refractory materials and heat insulation materials are combined, so that the heat dissipation loss and heat storage loss of a kiln body are reduced as much as possible, and the purposes of energy conservation and consumption reduction are achieved.
According to the operation mode of the industrial kiln, the method can be divided into an intermittent industrial kiln and a continuous industrial kiln. For a batch-type industrial furnace, the heat loss of the lining material includes heat dissipation loss and heat storage loss. With the development and technical progress of the heat insulation material, the low-heat-conduction nanometer heat insulation board is generally adopted as the heat insulation material, so that the temperature of the outer wall is reduced, and the heat dissipation loss is reduced. However, for high-temperature industrial kilns, when the temperature in the kiln is more than 1500 ℃, the total thermal resistance is increased due to the adoption of the nano thermal insulation plate, the temperature of the hot surface of the nano thermal insulation plate is increased, the nano thermal insulation plate is crystallized, the strength is reduced or the nano thermal insulation plate is pulverized, the structure of a thermal insulation layer of the industrial kiln is damaged, the expected effect of reducing the heat dissipation cannot be achieved, and the structure of a kiln lining is damaged due to the pulverization, so that safety accidents are caused. Therefore, the problem of high energy consumption of the industrial kiln can not be fundamentally solved by simply reducing the heat conductivity coefficient of the heat insulation material. In order to reduce the heat storage loss of the furnace lining material, the furnace lining material is made of light-weight refractory materials, and particularly, with the development of refractory raw materials such as microporous corundum, compact calcium hexaluminate and the like, the light weight of the furnace lining material of the high-temperature kiln becomes possible, and the heat storage loss of the furnace lining is greatly reduced. For example, in the patent technology of 'a lightweight corundum-spinel castable and a preparation method thereof' (CN 105236995), microporous corundum is adopted as a main aggregate to prepare the lightweight corundum-spinel castable with low thermal conductivity, and both the thermal conductivity and the bulk density are greatly reduced. However, the erosion and corrosion resistance of the lightweight refractory material against high temperature media (such as molten steel, steel slag, special atmosphere, etc.) at high temperature has not been verified, and the application of the lightweight refractory material in practical industrial kilns is limited.
In addition, the high-temperature industrial kiln which works intermittently has the furnace lining refractory material which is heated and cooled periodically, the temperature gradient generates thermal stress, the refractory material is cracked and peeled off under the action of thermal fatigue or thermal shock, and the service life of the furnace lining refractory material is reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a near-zero heat loss refractory material lining body of an intermittent operation high-temperature kiln with low heat loss and long service life of refractory materials of a lining and a preparation method thereof,
in order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the preparation method of the aluminum-silicon-nickel alloy @ alumina microcapsule, the aluminum-silicon-iron alloy @ alumina microcapsule and the aluminum-silicon alloy @ alumina microcapsule comprises the following steps:
alternately washing the aluminum-silicon-nickel alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 h at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the aluminum-silicon-nickel alloy powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the aluminum-silicon-nickel alloy @ alumina microcapsule.
Alternately washing the ferro-silicon-aluminum alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 hours at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the ferro-silicon-aluminum alloy @ aluminum oxide microcapsule.
Alternately washing the aluminum-silicon alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 h at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the aluminum-silicon alloy @ aluminum oxide microcapsule.
In the step 1, roasting is carried out in all six stages:
the first stage is as follows: heating the high-temperature atmosphere furnace from room temperature to 550-650 ℃ at the speed of 5-10 ℃/min; the furnace atmosphere is a water vapor atmosphere, and the water vapor: the inlet gauge pressure is 0.01-0.9 MPa, the temperature before the inlet is 110-300 ℃, and the flow rate is 3-5L/min.
And a second stage: and heating the high-temperature atmosphere furnace to 700-800 ℃ at the speed of 10-20 ℃/min, wherein the atmosphere in the furnace is air atmosphere.
And a third stage: heating the high-temperature atmosphere furnace to 850-950 ℃ at the speed of 5-8 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is 0.01-0.05 MPa.
A fourth stage: heating the high-temperature atmosphere furnace to 1050-1250 ℃ at the speed of 3-5 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is more than 0.05 and less than or equal to 0.1 MPa.
The fifth stage: heating the high-temperature atmosphere furnace to 1350-1500 ℃ at the speed of 5-10 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is more than 0.1 and less than or equal to 0.5 MPa.
The sixth stage: and (3) preserving the heat of the high-temperature atmosphere furnace for 30-180 min at 1350-1500 ℃, wherein the atmosphere in the furnace is air atmosphere.
Step 2, preparation methods of aluminum-silicon-nickel alloy @ ceramic macrocapsule, aluminum-silicon-iron alloy @ ceramic macrocapsule and aluminum-silicon alloy @ ceramic macrocapsule
And (3) placing the aluminum-silicon-nickel alloy ball into a ceramic spherical shell to obtain the aluminum-silicon-nickel alloy @ ceramic macrocapsule.
And placing the ferro-aluminum-silicon alloy ball into a ceramic spherical shell to obtain the ferro-aluminum-silicon alloy @ ceramic macrocapsule.
And (3) placing the aluminum-silicon alloy ball into a ceramic spherical shell to obtain the aluminum-silicon alloy @ ceramic macrocapsule.
The diameter of the alloy ball is 2-18 mm, and the alloy ball is one of an aluminum-silicon-nickel alloy ball, an aluminum-silicon-iron alloy ball and an aluminum-silicon alloy ball; the aluminum-silicon-nickel alloy ball, the aluminum-silicon-iron alloy ball and the aluminum-silicon alloy ball are respectively made of an aluminum-silicon-nickel alloy rod, an aluminum-silicon-iron alloy rod and an aluminum-silicon alloy rod which respectively correspond to each other.
Step 3, preparation method of high-temperature phase-change heat storage refractory material
55-65 wt% of aluminum-silicon-nickel alloy @ ceramic macrocapsule is used as an aggregate, 25-35 wt% of aluminum-silicon-nickel alloy @ alumina microcapsule and 4-6 wt% of α -Al2O3The micro powder, 0.1-1 wt% of silicon micro powder and 4-6 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the high-temperature phase change heat storage refractory material.
The phase-change temperature of the high-temperature phase-change heat-storage refractory material is 1150-1300 ℃.
Step 4, preparation method of intermediate-temperature phase-change heat storage refractory material
55-65 wt% of ferro-silicon-aluminum alloy @ ceramic macrocapsule is used as aggregate, 25-35 wt% of ferro-silicon-aluminum alloy @ alumina microcapsule and 4-6 wt% of α -Al2O3The micro powder, 0.1-1 wt% of silicon micro powder and 4-6 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing at 25-28 ℃ for 24-30 h with the relative air humidity of 75-80%, demolding, and drying at 110-300 ℃ for 24-36 h to obtain the intermediate-temperature phase-change heat-storage refractory material.
The phase-change temperature of the medium-temperature phase-change heat-storage refractory material is 800-950 ℃.
Step 5, preparation method of low-temperature phase-change heat storage refractory material
55-65 wt% of aluminum-silicon alloy @ ceramic macrocapsule is used as aggregate, 25-35 wt% of aluminum-silicon alloy @ alumina microcapsule and 4-6 wt% of α -Al2O3The micro powder, 0.1-1 wt% of silicon micro powder and 4-6 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the low-temperature phase change heat storage refractory material.
The phase-change temperature of the low-temperature phase-change heat-storage refractory material is 500-650 ℃.
Step 6, preparation method of batch-type operation high-temperature kiln near-zero heat loss refractory material lining body
The batch-type operation high-temperature kiln near-zero heat loss refractory material lining body sequentially comprises the following components from inside to outside along the thickness direction: working lining refractory material, permanent lining refractory material and heat insulating lining heat insulating material.
The working lining refractory material is positioned on a hot surface contacting a high-temperature medium in the kiln, and the thickness of the working lining refractory material is 150-250 mm.
The heat insulation lining and heat insulation material is a nanometer heat insulation plate, and the thickness of the heat insulation lining and heat insulation material is 5-20 mm.
The permanent lining refractory material is a phase change heat storage refractory material, and the phase change heat storage refractory material is composed of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material in sequence from inside to outside. Wherein:
the thickness of the high-temperature phase-change heat-storage refractory material is 30-80 mm.
The thickness of the medium-temperature phase-change heat storage refractory material is 20-60 mm.
The thickness of the low-temperature phase-change heat-storage refractory material is 30-110 mm.
The intermittently operated high-temperature kiln is one of a ladle, a torpedo tank, a ladle, a shuttle kiln and a down-draft kiln, and the refractory lining body comprises a top, a bottom and a wall body.
The preparation method of the ceramic spherical shell comprises the following steps:
the preparation method comprises the steps of ball-milling 80-90 wt% of corundum fine powder, 5-15 wt% of mullite fine powder, 3-5 wt% of α -alumina powder micro powder and 1-3 wt% of silica micro powder in a ball mill for 5-8 min to obtain mixed powder, adding 5-20 wt% of zirconia sol into the mixed powder, uniformly stirring to obtain mixed pug, forming the mixed pug by an injection molding machine to obtain a hemispherical shell mud blank with threads, drying the hemispherical shell mud blank with the threads at 110-180 ℃ for 24-36 h, heating to 1350-1650 ℃ at the speed of 3-5 ℃/min, and preserving heat for 2-4 h to obtain the ceramic hemispherical shell with the threads.
The ceramic hemispherical shell with the threads is a ceramic hemispherical shell with internal threads and a ceramic hemispherical shell with external threads; the ceramic hemispherical shell with the internal thread and the ceramic hemispherical shell with the external thread are connected into a hollow sphere through the thread, and the ceramic spherical shell is obtained.
The annular inner wall of the edge of the hemispherical ceramic shell with the internal thread is provided with the internal thread, and the annular outer wall of the edge of the hemispherical ceramic shell with the external thread is provided with the external thread. The ceramic hemispherical shell with the internal thread and the ceramic hemispherical shell with the external thread have the same outer diameter and wall thickness; the wall thickness is 0.6-2 mm, and the outer diameter is 3.5-24 mm; the nominal diameter of the internal thread and the external thread is 2.7-21 mm.
Al of the corundum fine powder2O3The content is more than or equal to 98 wt%; the grain size of the corundum fine powder is less than or equal to 15 mu m;
the mullite fine powder comprises the following components: al (Al)2O3The content is more than or equal to 70wt percent, and SiO is2The content is more than or equal to 22 wt%; the grain diameter of the mullite fine powder is less than or equal to 15 mu m;
the zirconium dioxide sol has a solid content of 30 wt% and a particle size of 20-50 nm.
The aluminum silicon nickel alloy rod comprises the following chemical components: 17-25 wt% of Al, 53-60 wt% of Si and 20-28 wt% of Ni; the aluminum-silicon-nickel alloy powder and the aluminum-silicon-nickel alloy rod have the same chemical components, and the particle size of the aluminum-silicon-nickel alloy powder is 13-250 mu m.
The aluminum-silicon-iron alloy rod comprises the following chemical components: the Al content is 40-45 wt%, the Si content is 40-45 wt%, and the Fe content is 10-15 wt%; the aluminum-silicon-iron alloy powder and the aluminum-silicon-iron alloy rod have the same chemical composition, and the particle size of the aluminum-silicon-iron alloy powder is 13-250 mu m.
The Si content of the aluminum-silicon alloy rod is 12-45 wt%; the silicon content of the aluminum-silicon alloy powder is the same as that of the aluminum-silicon alloy rod, and the particle size of the aluminum-silicon alloy powder is 13-250 mu m.
The α -Al2O3Micronized Al2O3Content is more than or equal to 97wt percent, α -Al2O3The particle size of the micro powder is less than or equal to 8 mu m.
SiO of the silicon micropowder2Content (wt.)>92 wt%; particle size of silica micropowder<1μm。
The chemical components of the calcium aluminate cement are as follows: al (Al)2O350-60 wt% of SiO2Content (wt.)<8wt％，Fe2O3Content (wt.)<2.5 wt%; the grain diameter of the calcium aluminate cement is less than or equal to 10 mu m.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
the permanent lining refractory material adopted by the invention is a phase change heat storage refractory material which is composed of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material which are prepared according to the temperature gradient from high temperature to low temperature, and relatively stable temperature distribution is formed in the furnace lining, so that the temperature fluctuation of the working lining refractory material in the processes of heating and cooling is reduced, and the service life is prolonged. In the phase-change heat-storage refractory material, the alloy @ alumina ceramic macrocapsule is used as an aggregate, and the alloy @ alumina microcapsule is used as a matrix, so that heat is stored to the maximum extent. The heat insulation layer is matched with a nanometer heat insulation plate with low heat conductivity coefficient, so that the temperature of the shell of the intermittent operation high-temperature kiln is close to the ambient temperature, the heat loss is close to zero, and the near-zero heat loss is realized.
The working process of the invention is as follows:
let room temperature be t0The maximum working temperature of the intermittent operation high-temperature kiln is thThe phase transition temperature of the aluminum-silicon alloy, the aluminum-silicon-iron alloy and the aluminum-silicon-nickel alloy in the phase transition heat storage refractory material is tcl、tcmAnd tchAnd t iscl<tcm<tch. In the temperature rising-reducing process in one working period of the intermittent operation high-temperature kiln, ThFor intermittent operation of the temperature profile in a high-temperature kiln, T1-2High temperature phase change heat storage refractory material as working lining and permanent lining interface temperature change curve, T2-3Temperature change curve, T, of interface between high-temperature phase change heat storage refractory and medium-temperature phase change heat storage refractory as permanent lining3-4Is the temperature change curve T of the interface of the intermediate-temperature phase-change heat-storage refractory material and the low-temperature phase-change heat-storage refractory material4-5Is a temperature change curve of the interface between the permanent lining low-temperature phase change heat storage refractory material and the heat insulation lining, T5-SIs the temperature change curve of the interface of the heat insulation lining and the steel shell, TwIs a temperature change curve of the high-temperature kiln shell.
According to the characteristics of transient heat transfer, in the temperature rising and reducing processes of the intermittent operation high-temperature kiln, the temperature distribution change in the refractory material of the furnace lining is as follows:
in the temperature rising process, the temperature of the working lining and the temperature of the permanent lining are sequentially raised along with the temperature rise in the furnace, and when the temperature of the high-temperature phase-change heat-storage refractory material of the permanent lining is raised to the phase-change temperature t of the aluminum-silicon-nickel alloychWhen the heat-insulating lining is used, the aluminum-silicon-nickel alloy generates phase change to absorb heat, and at the moment, the temperature of the medium-temperature phase change heat storage material, the temperature of the low-temperature phase change heat storage material, the temperature of the heat-insulating lining and the temperature T of the outer wall are controlledwAll remain unchanged; similarly, when the high-temperature phase-change alloy is completely subjected to phase change, the heat storage reaches saturation, and the temperature of the medium-temperature phase-change heat storage refractory material is increased to be higher than the phase-change temperature t of the sendust alloycmDuring the process, the Al-Si-Fe alloy generates phase change, the temperature of the low-temperature phase change heat storage material, the temperature of the heat insulation lining and the temperature T of the outer wallwKeeping the same;when the medium-temperature phase-change alloy is completely subjected to phase change, the heat storage reaches saturation, and the temperature of the low-temperature phase-change heat storage refractory material is increased to be higher than the phase-change temperature t of the aluminum-silicon alloyclWhen the aluminum-silicon alloy is in phase transition, the temperature of the heat insulation lining and the temperature T of the outer wallwKeeping the same; the heat storage of the low-temperature phase-change heat-storage refractory material reaches saturation along with the rise of the temperature in the kiln, and the highest interface temperature of the heat-insulation layer is the phase-change temperature t of the aluminum-silicon alloycl. Because the maximum service temperature of the nanometer thermal insulation board is more than tclAnd the heat-insulating layer nanometer heat-insulating plate has low heat conductivity coefficient and large heat resistance, so that the temperature of the shell is basically kept unchanged.
According to a heat dissipation calculation formula: q ═ K (t)w-t0) Wherein: k is a heat exchange coefficient and is related to the temperature of the outer wall when the temperature t of the outer wall iswAnd ambient temperature t0When the phase difference is not large, the heat exchange coefficient K is low; q is heat dissipation when the temperature of the housing is twAnd ambient temperature t0When the temperature difference is close to 0, the heat dissipation is almost 0, and the heat loss is approximate to zero.
In the intermittent operation high-temperature kiln cooling process, the temperature of the working lining is firstly reduced, and the working lining is a permanent lining and a heat insulation lining in sequence. When the temperature of the high-temperature phase-change heat-storage refractory material of the permanent lining is lower than the phase-change temperature t of the aluminum-silicon-nickel alloychDuring the process, the aluminum-silicon-nickel alloy generates phase change heat release, delays the reduction speed of the temperature of the working lining, and keeps the temperature t of the shellwAnd is not changed. With the continuous decrease of the temperature in the intermittent high-temperature kiln, the temperature of the medium-temperature phase-change heat-storage refractory material of the permanent lining is lower than the phase-change temperature t of the ferro-aluminum-silicon alloycmDuring the process, the Al-Si-Fe alloy generates phase change heat release, delays the reduction speed of the temperature of the working lining and the temperature of the high-temperature phase change heat storage refractory material of the permanent lining, and keeps the temperature t of the shellwAnd is not changed. With the continuous reduction of the temperature in the intermittent operation high-temperature kiln, the temperature of the low-temperature phase-change heat-storage refractory material of the permanent lining is lower than the phase-change temperature t of the aluminum-silicon alloyclDuring the process, the aluminum-silicon alloy generates phase change heat release, delays the reduction speed of the temperature of the working lining, the temperature of the high-temperature phase change heat storage refractory material of the permanent lining and the temperature of the medium-temperature phase change heat storage refractory material of the permanent lining, and keeps the temperature t of the shellwAnd is not changed. Is connected withIs close to the ambient temperature t0Approximately zero heat loss.
According to the temperature change curve in the intermittent operation high-temperature kiln, the thicknesses of three different phase-change heat-storage refractory materials and the thickness of a heat insulation layer are designed by utilizing the difference of phase-change temperature and phase-change enthalpy in the three phase-change heat-storage refractory materials of the permanent lining through heat transfer calculation, so that the stable temperature of the shell is realized, the temperature is close to the ambient temperature, and the heat loss is approximately zero; meanwhile, the temperature drop speed of the working lining and the temperature fluctuation of the shell and the heat insulation layer are delayed, the stress change of the working lining and the heat insulation lining is reduced, the shell is prevented from deforming, and the structural integrity and the long service life of the high-temperature kiln body of the high-temperature kiln are ensured.
The main performance parameters of the near-zero heat loss refractory material lining body of the intermittent operation high-temperature kiln prepared by the invention are as follows:
high-temperature phase-change heat storage refractory material: the bulk density is 3.12 to 3.86g/cm3(ii) a The thermal conductivity (1000-1200 ℃) is 1.52-1.78W/(m DEG C); the heat storage density (1150-1300 ℃) is 260.2-380.8J/g; the compressive strength is 60-115 MPa; the compressive strength of 30 times of air cooling during thermal shock (1200 ℃) is 25-60 MPa.
Intermediate-temperature phase-change heat storage refractory material: the bulk density is 2.62-3.36 g/cm3(ii) a The heat conductivity coefficient (600-800 ℃) is 1.23-1.56W/(m DEG C); the heat storage density (800-950 ℃) is 180.2-240.8J/g; the compressive strength is 80-125 MPa; the compressive strength of 30 times of air cooling in thermal shock (800 ℃) is 15-40 MPa.
Low-temperature phase-change heat storage refractory material: the bulk density is 2.02-2.56 g/cm3(ii) a The thermal conductivity (300-600 ℃) is 1.63-1.85W/(m DEG C); the heat storage density (500-650 ℃) is 110.2-180.8J/g; the compressive strength is 70-120 MPa; the compressive strength of 30 times of air cooling after thermal shock (600 ℃) is 30-70 MPa.
Therefore, the near-zero heat loss refractory material lining body of the intermittent operation high-temperature kiln prepared by the invention has the characteristics that the heat loss is similar to zero and the service life of the refractory material of the furnace lining is long.
Drawings
FIG. 1 is a graph of the temperature change of a near zero heat loss refractory lining of an intermittently operated high temperature kiln of the present invention.
Detailed Description
The following further description of the present group of inventions, with reference to the drawings and detailed description, is not intended to limit the scope of the inventions.
In this embodiment:
the refractory lining body comprises a top, a bottom and a wall body.
The preparation method of the ceramic spherical shell comprises the following steps:
the preparation method comprises the steps of ball-milling 80-90 wt% of corundum fine powder, 5-15 wt% of mullite fine powder, 3-5 wt% of α -alumina powder micro powder and 1-3 wt% of silica micro powder in a ball mill for 5-8 min to obtain mixed powder, adding 5-20 wt% of zirconia sol into the mixed powder, uniformly stirring to obtain mixed pug, forming the mixed pug by an injection molding machine to obtain a hemispherical shell mud blank with threads, drying the hemispherical shell mud blank with the threads at 110-180 ℃ for 24-36 h, heating to 1350-1650 ℃ at the speed of 3-5 ℃/min, and preserving heat for 2-4 h to obtain the ceramic hemispherical shell with the threads.
The ceramic hemispherical shell with the threads is a ceramic hemispherical shell with internal threads and a ceramic hemispherical shell with external threads; the ceramic hemispherical shell with the internal thread and the ceramic hemispherical shell with the external thread are connected into a hollow sphere through the thread, and the ceramic spherical shell is obtained.
The inner thread is arranged on the annular inner wall at the edge of the hemispherical ceramic shell with the inner thread, and the outer thread is arranged on the annular outer wall at the edge of the hemispherical ceramic shell with the outer thread; the ceramic hemispherical shell with the internal thread and the ceramic hemispherical shell with the external thread have the same outer diameter and wall thickness. The wall thickness is 0.6-2 mm, and the outer diameter is 3.5-24 mm; the nominal diameter of the internal thread and the external thread is 2.7-21 mm.
Al of the corundum fine powder2O3The content is more than or equal to 98 wt%; the grain size of the corundum fine powder is less than or equal to 15 mu m;
the mullite fine powder comprises the following components: al (Al)2O3The content is more than or equal to 70wt％，SiO2The content is more than or equal to 22 wt%; the grain diameter of the mullite fine powder is less than or equal to 15 mu m;
the zirconium dioxide sol has a solid content of 30 wt% and a particle size of 20-50 nm.
The aluminum silicon nickel alloy rod comprises the following chemical components: 17-25 wt% of Al, 53-60 wt% of Si and 20-28 wt% of Ni; the aluminum-silicon-nickel alloy powder and the aluminum-silicon-nickel alloy rod have the same chemical components, and the particle size of the aluminum-silicon-nickel alloy powder is 13-250 mu m.
The aluminum-silicon-iron alloy rod comprises the following chemical components: the Al content is 40-45 wt%, the Si content is 40-45 wt%, and the Fe content is 10-15 wt%; the aluminum-silicon-iron alloy powder and the aluminum-silicon-iron alloy rod have the same chemical composition, and the particle size of the aluminum-silicon-iron alloy powder is 13-250 mu m.
The Si content of the aluminum-silicon alloy rod is 12-45 wt%; the silicon content of the aluminum-silicon alloy powder is the same as that of the aluminum-silicon alloy rod, and the particle size of the aluminum-silicon alloy powder is 13-250 mu m.
The α -Al2O3Micronized Al2O3Content is more than or equal to 97wt percent, α -Al2O3The particle size of the micro powder is less than or equal to 8 mu m.
SiO of the silicon micropowder2Content (wt.)>92 wt%; particle size of silica micropowder<1μm。
The chemical components of the calcium aluminate cement are as follows: al (Al)2O350-60 wt% of SiO2Content (wt.)<8wt％，Fe2O3Content (wt.)<2.5 wt%; the grain diameter of the calcium aluminate cement is less than or equal to 10 mu m.
Example 1
A refractory material lining body with near zero heat loss for intermittently operating a high-temperature kiln and a preparation method thereof. The preparation method comprises the following steps:
the preparation method of the aluminum-silicon-nickel alloy @ alumina microcapsule, the aluminum-silicon-iron alloy @ alumina microcapsule and the aluminum-silicon alloy @ alumina microcapsule comprises the following steps:
alternately washing the aluminum-silicon-nickel alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 h at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the aluminum-silicon-nickel alloy powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the aluminum-silicon-nickel alloy @ alumina microcapsule.
Alternately washing the ferro-silicon-aluminum alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 hours at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the ferro-silicon-aluminum alloy @ aluminum oxide microcapsule.
Alternately washing the aluminum-silicon alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 h at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the aluminum-silicon alloy @ aluminum oxide microcapsule.
In the step 1, roasting is carried out in all six stages:
the first stage is as follows: heating the high-temperature atmosphere furnace from room temperature to 550-650 ℃ at the speed of 5-10 ℃/min; the furnace atmosphere is a water vapor atmosphere, and the water vapor: the inlet gauge pressure is 0.01-0.9 MPa, the temperature before the inlet is 110-300 ℃, and the flow rate is 3-5L/min.
And a second stage: and heating the high-temperature atmosphere furnace to 700-800 ℃ at the speed of 10-20 ℃/min, wherein the atmosphere in the furnace is air atmosphere.
And a third stage: heating the high-temperature atmosphere furnace to 850-950 ℃ at the speed of 5-8 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is 0.01-0.05 MPa.
A fourth stage: heating the high-temperature atmosphere furnace to 1050-1250 ℃ at the speed of 3-5 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is more than 0.05 and less than or equal to 0.1 MPa.
The fifth stage: heating the high-temperature atmosphere furnace to 1350-1500 ℃ at the speed of 5-10 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is more than 0.1 and less than or equal to 0.5 MPa.
The sixth stage: and (3) preserving the heat of the high-temperature atmosphere furnace for 30-180 min at 1350-1500 ℃, wherein the atmosphere in the furnace is air atmosphere.
Step 2, preparation methods of aluminum-silicon-nickel alloy @ ceramic macrocapsule, aluminum-silicon-iron alloy @ ceramic macrocapsule and aluminum-silicon alloy @ ceramic macrocapsule
And (3) placing the aluminum-silicon-nickel alloy ball into a ceramic spherical shell to obtain the aluminum-silicon-nickel alloy @ ceramic macrocapsule.
And placing the ferro-aluminum-silicon alloy ball into a ceramic spherical shell to obtain the ferro-aluminum-silicon alloy @ ceramic macrocapsule.
And (3) placing the aluminum-silicon alloy ball into a ceramic spherical shell to obtain the aluminum-silicon alloy @ ceramic macrocapsule.
The diameter of the alloy ball is 2-18 mm, and the alloy ball is one of an aluminum-silicon-nickel alloy ball, an aluminum-silicon-iron alloy ball and an aluminum-silicon alloy ball; the aluminum-silicon-nickel alloy ball, the aluminum-silicon-iron alloy ball and the aluminum-silicon alloy ball are respectively made of an aluminum-silicon-nickel alloy rod, an aluminum-silicon-iron alloy rod and an aluminum-silicon alloy rod which respectively correspond to each other.
Step 3, preparation method of high-temperature phase-change heat storage refractory material
55-59 wt% of aluminum-silicon-nickel alloy @ ceramic macrocapsule is used as an aggregate, 31-35 wt% of aluminum-silicon-nickel alloy @ alumina microcapsule and 4-5 wt% of α -Al2O3The micro powder, 0.1-0.6 wt% of silicon micro powder and 5-6 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the high-temperature phase change heat storage refractory material.
The phase-change temperature of the high-temperature phase-change heat-storage refractory material is 1150-1300 ℃.
Step 4, preparation method of intermediate-temperature phase-change heat storage refractory material
58-62 wt% of sendust @ ceramic macrocapsule is used as aggregate, 28-32 wt% of sendust @ alumina microcapsule and 4.5-5.5 wt% of α -Al2O3Micro powder, 0.3-0.8 wt% of silicon micro powder and 4.5-5.5 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; then mixing the pre-mixed matrix material withMixing the aggregates, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 h at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 h at the temperature of 110-300 ℃ to obtain the intermediate-temperature phase-change heat-storage refractory material.
The phase-change temperature of the medium-temperature phase-change heat-storage refractory material is 800-950 ℃.
Step 5, preparation method of low-temperature phase-change heat storage refractory material
61-65 wt% of aluminum-silicon alloy @ ceramic macrocapsule is used as aggregate, 25-29 wt% of aluminum-silicon alloy @ alumina microcapsule and 5-6 wt% of α -Al2O3Micro powder, 0.5-1.0 wt% of silicon micro powder and 4-5 wt% of calcium aluminate cement are used as matrixes, and the sum of aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the low-temperature phase change heat storage refractory material.
The phase-change temperature of the low-temperature phase-change heat-storage refractory material is 500-650 ℃.
Step 6, preparation method of batch-type operation high-temperature kiln near-zero heat loss refractory material lining body
The batch-type operation high-temperature kiln near-zero heat loss refractory material lining body sequentially comprises the following components from inside to outside along the thickness direction: working lining refractory material, permanent lining refractory material and heat insulating lining heat insulating material.
The working lining refractory material is positioned on a hot surface contacting molten steel and steel slag, and the thickness of the working lining refractory material is 200-250 mm.
The heat insulation lining and heat insulation material is a nanometer heat insulation plate, and the thickness of the heat insulation lining and heat insulation material is 15-20 mm.
The permanent lining refractory material is a phase change heat storage refractory material, and the phase change heat storage refractory material is composed of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material in sequence from inside to outside. Wherein:
the thickness of the high-temperature phase-change heat-storage refractory material is 50-80 mm.
The thickness of the medium-temperature phase-change heat storage refractory material is 40-60 mm.
The thickness of the low-temperature phase-change heat-storage refractory material is 30-60 mm.
The intermittent operation high-temperature kiln is a ladle.
Example 2
A refractory material lining body with near zero heat loss for intermittently operating a high-temperature kiln and a preparation method thereof. The preparation method comprises the following steps:
step 1 was the same as step 1 of example 1.
Step 2 was the same as step 2 of example 1.
Step 3, preparation method of high-temperature phase-change heat storage refractory material
58-62 wt% of aluminum-silicon-nickel alloy @ ceramic macrocapsule is used as an aggregate, 28-32 wt% of aluminum-silicon-nickel alloy @ alumina microcapsule and 4.5-5.5 wt% of α -Al2O3Micro powder, 0.3-0.8 wt% of silicon micro powder and 4.5-5.5 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the high-temperature phase change heat storage refractory material.
The phase-change temperature of the high-temperature phase-change heat-storage refractory material is 1150-1300 ℃.
Step 4, preparation method of intermediate-temperature phase-change heat storage refractory material
61-65 wt% of ferro-silicon-aluminum alloy @ ceramic macrocapsule is used as aggregate, 25-29 wt% of ferro-silicon-aluminum alloy @ alumina microcapsule and 5-6 wt% of α -Al2O3Micro powder, 0.5-1.0 wt% of silicon micro powder and 4-5 wt% of calcium aluminate cement are used as matrixes, and the sum of aggregate and the matrixes is used as raw materials. Firstly, uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materialsUniformly mixing to obtain a premixed matrix material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing at 25-28 ℃ for 24-30 h with the relative air humidity of 75-80%, demolding, and drying at 110-300 ℃ for 24-36 h to obtain the intermediate-temperature phase-change heat-storage refractory material.
The phase-change temperature of the medium-temperature phase-change heat-storage refractory material is 800-950 ℃. .
Step 5, preparation method of low-temperature phase-change heat storage refractory material
55-59 wt% of aluminum-silicon alloy @ ceramic macrocapsule is used as aggregate, 31-35 wt% of aluminum-silicon alloy @ alumina microcapsule and 4-5 wt% of α -Al2O3The micro powder, 0.1-0.6 wt% of silicon micro powder and 5-6 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the low-temperature phase change heat storage refractory material.
The phase-change temperature of the low-temperature phase-change heat-storage refractory material is 500-650 ℃.
Step 6, preparation method of batch-type operation high-temperature kiln near-zero heat loss refractory material lining body
The batch-type operation high-temperature kiln near-zero heat loss refractory material lining body sequentially comprises the following components from inside to outside along the thickness direction: working lining refractory material, permanent lining refractory material and heat insulating lining heat insulating material.
The working lining refractory material is positioned on a hot surface contacting high-temperature gas in the kiln, and the thickness of the working lining refractory material is 170-230 mm.
The heat insulation lining and heat insulation material is a nanometer heat insulation plate, and the thickness of the heat insulation lining and heat insulation material is 10-15 mm.
The permanent lining refractory material is a phase change heat storage refractory material, and the phase change heat storage refractory material is composed of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material in sequence from inside to outside. Wherein:
the thickness of the high-temperature phase-change heat-storage refractory material is 45-65 mm.
The thickness of the medium-temperature phase-change heat storage refractory material is 30-50 mm.
The thickness of the low-temperature phase-change heat-storage refractory material is 50-80 mm.
The intermittent operation high-temperature kiln is a shuttle kiln.
Example 3
A refractory material lining body with near zero heat loss for intermittently operating a high-temperature kiln and a preparation method thereof. The preparation method comprises the following steps:
step 1 was the same as step 1 of example 1.
Step 2 was the same as step 2 of example 1.
Step 3, preparation method of high-temperature phase-change heat storage refractory material
61-65 wt% of aluminum-silicon-nickel alloy @ ceramic macrocapsule is used as aggregate, 25-29 wt% of aluminum-silicon-nickel alloy @ alumina microcapsule and 5-6 wt% of α -Al2O3Micro powder, 0.5-1.0 wt% of silicon micro powder and 4-5 wt% of calcium aluminate cement are used as matrixes, and the sum of aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the high-temperature phase change heat storage refractory material.
The phase-change temperature of the high-temperature phase-change heat-storage refractory material is 1150-1300 ℃.
Step 4, preparation method of intermediate-temperature phase-change heat storage refractory material
55-59 wt% of ferro-silicon-aluminum alloy @ ceramic macrocapsule is used as aggregate, 31-35 wt% of ferro-silicon-aluminum alloy @ alumina microcapsule and 4-5 wt% of α -Al2O3The micro powder, 0.1-0.6 wt% of silicon micro powder and 5-6 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials.Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing at 25-28 ℃ for 24-30 h with the relative air humidity of 75-80%, demolding, and drying at 110-300 ℃ for 24-36 h to obtain the intermediate-temperature phase-change heat-storage refractory material.
The phase-change temperature of the medium-temperature phase-change heat-storage refractory material is 800-950 ℃. .
Step 5, preparation method of low-temperature phase-change heat storage refractory material
58-62 wt% of aluminum-silicon alloy @ ceramic macrocapsule is used as an aggregate, 28-32 wt% of aluminum-silicon alloy @ alumina microcapsule and 4.5-5.5 wt% of α -Al2O3Micro powder, 0.3-0.8 wt% of silicon micro powder and 4.5-5.5 wt% of calcium aluminate cement are used as matrixes, and the sum of the aggregate and the matrixes is used as raw materials. Uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; and mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing for 24-30 hours at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and drying for 24-36 hours at the temperature of 110-300 ℃ to obtain the low-temperature phase change heat storage refractory material.
The phase-change temperature of the low-temperature phase-change heat-storage refractory material is 500-650 ℃.
Step 6, preparation method of batch-type operation high-temperature kiln near-zero heat loss refractory material lining body
The batch-type operation high-temperature kiln near-zero heat loss refractory material lining body sequentially comprises the following components from inside to outside along the thickness direction: working lining refractory material, permanent lining refractory material and heat insulating lining heat insulating material.
The working lining refractory material is positioned on a hot surface contacting molten iron or iron slag in the kiln, and the thickness of the working lining refractory material is 150-200 mm.
The heat insulation lining and heat insulation material is a nanometer heat insulation plate, and the thickness of the heat insulation lining and heat insulation material is 5-10 mm.
The permanent lining refractory material is a phase change heat storage refractory material, and the phase change heat storage refractory material is composed of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material in sequence from inside to outside. Wherein:
the thickness of the high-temperature phase-change heat-storage refractory material is 30-45 mm.
The thickness of the medium-temperature phase-change heat storage refractory material is 20-40 mm.
The thickness of the low-temperature phase-change heat-storage refractory material is 80-110 mm.
The intermittent operation high-temperature kiln is a ladle.
Compared with the prior art, the specific implementation mode has the following positive effects:
the permanent lining refractory material adopted by the embodiment is a phase change heat storage refractory material consisting of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material which are prepared from different phase change temperatures according to a temperature gradient from high temperature to low temperature, relatively stable temperature distribution is formed in a furnace lining, temperature fluctuation of the working lining refractory material in the processes of temperature rise and temperature drop is reduced, and the service life is prolonged. In the phase-change heat-storage refractory material, the alloy @ alumina ceramic macrocapsule is used as an aggregate, and the alloy @ alumina microcapsule is used as a matrix, so that heat is stored to the maximum extent. The heat insulation layer is matched with a nanometer heat insulation plate with low heat conductivity coefficient, so that the temperature of the shell of the intermittent operation high-temperature kiln is close to the ambient temperature, the heat loss is close to zero, and the near-zero heat loss is realized.
The working process of the specific embodiment is as follows:
let room temperature be t0The maximum working temperature of the intermittent operation high-temperature kiln is thThe phase transition temperature of the aluminum-silicon alloy, the aluminum-silicon-iron alloy and the aluminum-silicon-nickel alloy in the phase transition heat storage refractory material is tcl、tcmAnd tchAnd t iscl<tcm<tch. In the temperature rising-reducing process in one working period of the intermittent operation high-temperature kiln, ThFor intermittent operation of the temperature profile in a high-temperature kiln, T1-2High temperature phase change heat storage refractory material as working lining and permanent lining interface temperature change curve, T2-3Temperature change curve, T, of interface between high-temperature phase change heat storage refractory and medium-temperature phase change heat storage refractory as permanent lining3-4Is the temperature change curve T of the interface of the intermediate-temperature phase-change heat-storage refractory material and the low-temperature phase-change heat-storage refractory material4-5Is a temperature change curve of the interface between the permanent lining low-temperature phase change heat storage refractory material and the heat insulation lining, T5-SIs the temperature change curve of the interface of the heat insulation lining and the steel shell, TwIs a temperature change curve of the high-temperature kiln shell.
According to the characteristics of transient heat transfer, during the temperature rising and lowering process of the intermittently operated high-temperature kiln, the temperature distribution change in the refractory material of the furnace lining is as shown in fig. 1, fig. 1 is a temperature change curve diagram of the near-zero heat loss refractory material lining of the intermittently operated high-temperature kiln of the embodiment 1, and as can be seen from fig. 1: in the temperature rising process, the temperature of the working lining and the temperature of the permanent lining are sequentially raised along with the temperature rise in the furnace, and when the temperature of the high-temperature phase-change heat-storage refractory material of the permanent lining is raised to the phase-change temperature t of the aluminum-silicon-nickel alloychWhen the heat-insulating lining is used, the aluminum-silicon-nickel alloy generates phase change to absorb heat, and at the moment, the temperature of the medium-temperature phase change heat storage material, the temperature of the low-temperature phase change heat storage material, the temperature of the heat-insulating lining and the temperature T of the outer wall are controlledwAll remain unchanged; similarly, when the high-temperature phase-change alloy is completely subjected to phase change, the heat storage reaches saturation, and the temperature of the medium-temperature phase-change heat storage refractory material is increased to be higher than the phase-change temperature t of the sendust alloycmDuring the process, the Al-Si-Fe alloy generates phase change, the temperature of the low-temperature phase change heat storage material, the temperature of the heat insulation lining and the temperature T of the outer wallwKeeping the same; when the medium-temperature phase-change alloy is completely subjected to phase change, the heat storage reaches saturation, and the temperature of the low-temperature phase-change heat storage refractory material is increased to be higher than the phase-change temperature t of the aluminum-silicon alloyclWhen the aluminum-silicon alloy is in phase transition, the temperature of the heat insulation lining and the temperature T of the outer wallwKeeping the same; the heat storage of the low-temperature phase-change heat-storage refractory material reaches saturation along with the rise of the temperature in the kiln, and the highest interface temperature of the heat-insulation layer is the phase-change temperature t of the aluminum-silicon alloycl. Because the maximum service temperature of the nanometer thermal insulation board is more than tclAnd the heat-insulating layer nanometer heat-insulating plate has low heat conductivity coefficient and large heat resistance, so that the temperature of the shell is basically kept unchanged.
According toThe heat dissipation calculation formula is as follows: q ═ K (t)w-t0) Wherein: k is a heat exchange coefficient and is related to the temperature of the outer wall when the temperature t of the outer wall iswAnd ambient temperature t0When the phase difference is not large, the heat exchange coefficient K is low; q is heat dissipation when the temperature of the housing is twAnd ambient temperature t0When the temperature difference is close to 0, the heat dissipation capacity is almost 0, and the heat loss is approximately zero.
In the intermittent operation high-temperature kiln cooling process, the temperature of the working lining is firstly reduced, and the working lining is a permanent lining and a heat insulation lining in sequence. When the temperature of the high-temperature phase-change heat-storage refractory material of the permanent lining is lower than the phase-change temperature t of the aluminum-silicon-nickel alloychDuring the process, the aluminum-silicon-nickel alloy generates phase change heat release, delays the reduction speed of the temperature of the working lining, and keeps the temperature t of the shellwAnd is not changed. With the continuous decrease of the temperature in the intermittent high-temperature kiln, the temperature of the medium-temperature phase-change heat-storage refractory material of the permanent lining is lower than the phase-change temperature t of the ferro-aluminum-silicon alloycmDuring the process, the Al-Si-Fe alloy generates phase change heat release, delays the reduction speed of the temperature of the working lining and the temperature of the high-temperature phase change heat storage refractory material of the permanent lining, and keeps the temperature t of the shellwAnd is not changed. With the continuous reduction of the temperature in the intermittent operation high-temperature kiln, the temperature of the low-temperature phase-change heat-storage refractory material of the permanent lining is lower than the phase-change temperature t of the aluminum-silicon alloyclDuring the process, the aluminum-silicon alloy generates phase change heat release, delays the reduction speed of the temperature of the working lining, the temperature of the high-temperature phase change heat storage refractory material of the permanent lining and the temperature of the medium-temperature phase change heat storage refractory material of the permanent lining, and keeps the temperature t of the shellwAnd is not changed. Close to the ambient temperature t0Approximately zero heat loss.
According to the temperature change curve in the intermittent operation high-temperature kiln, the thickness of three different phase-change heat-storage refractory materials and the thickness of a heat insulation layer are designed by utilizing the difference of phase-change temperature and phase-change enthalpy in the three phase-change heat-storage refractory materials of the permanent lining through heat transfer calculation, so that the temperature of the shell is stable and is close to the ambient temperature, and the heat loss is approximately zero; meanwhile, the temperature drop speed of the working lining and the temperature fluctuation of the shell and the heat insulation layer are delayed, the stress change of the working lining and the heat insulation lining is reduced, the shell is prevented from deforming, and the structural integrity and the long service life of the high-temperature kiln body of the high-temperature kiln are ensured.
The batch-type operation high-temperature kiln near-zero heat loss refractory material lining body prepared by the specific embodiment has the main performance parameters as follows:
high-temperature phase-change heat storage refractory material: the bulk density is 3.12 to 3.86g/cm3(ii) a The thermal conductivity (1000-1200 ℃) is 1.52-1.78W/(m DEG C); the heat storage density (1150-1300 ℃) is 260.2-380.8J/g; the compressive strength is 60-115 MPa; the compressive strength of 30 times of air cooling during thermal shock (1200 ℃) is 25-60 MPa.
Intermediate-temperature phase-change heat storage refractory material: the bulk density is 2.62-3.36 g/cm3(ii) a The heat conductivity coefficient (600-800 ℃) is 1.23-1.56W/(m DEG C); the heat storage density (800-950 ℃) is 180.2-240.8J/g; the compressive strength is 80-125 MPa; the compressive strength of 30 times of air cooling in thermal shock (800 ℃) is 15-40 MPa.
Low-temperature phase-change heat storage refractory material: the bulk density is 2.02-2.56 g/cm3(ii) a The thermal conductivity (300-600 ℃) is 1.63-1.85W/(m DEG C); the heat storage density (500-650 ℃) is 110.2-180.8J/g; the compressive strength is 70-120 MPa; the compressive strength of 30 times of air cooling after thermal shock (600 ℃) is 30-70 MPa.
Therefore, the near-zero heat loss refractory lining of the batch operation high-temperature kiln prepared by the embodiment has the characteristics of approximate zero heat loss and long service life of the refractory material of the furnace lining.

Claims (9)

1. A method for preparing a near-zero heat loss refractory material lining body of a batch-type operation high-temperature kiln is characterized by comprising the following steps:
the preparation method of the aluminum-silicon-nickel alloy @ alumina microcapsule, the aluminum-silicon-iron alloy @ alumina microcapsule and the aluminum-silicon alloy @ alumina microcapsule comprises the following steps:
alternately washing the aluminum-silicon-nickel alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 h at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the aluminum-silicon-nickel alloy powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain an aluminum-silicon-nickel alloy @ alumina microcapsule;
alternately washing the ferro-silicon-aluminum alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 hours at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the washed ferro-silicon-aluminum alloy powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain the ferro-silicon-aluminum alloy @ aluminum oxide microcapsule;
alternately washing the aluminum-silicon alloy powder with alkali and deionized water for 3-5 times, drying for 8-12 h at the temperature of 60-110 ℃ in a nitrogen atmosphere, then placing the aluminum-silicon alloy powder in a high-temperature atmosphere furnace, roasting according to six stages, and naturally cooling to obtain an aluminum-silicon alloy @ aluminum oxide microcapsule;
in the step 1, roasting is carried out in all six stages:
the first stage is as follows: heating the high-temperature atmosphere furnace from room temperature to 550-650 ℃ at the speed of 5-10 ℃/min; the furnace atmosphere is a water vapor atmosphere, and the water vapor: the inlet gauge pressure is 0.01-0.9 MPa, the temperature before the inlet is 110-300 ℃, and the flow rate is 3-5L/min;
and a second stage: heating the high-temperature atmosphere furnace to 700-800 ℃ at the speed of 10-20 ℃/min, wherein the atmosphere in the furnace is air atmosphere;
and a third stage: heating the high-temperature atmosphere furnace to 850-950 ℃ at the speed of 5-8 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is 0.01-0.05 MPa;
a fourth stage: heating the high-temperature atmosphere furnace to 1050-1250 ℃ at the speed of 3-5 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is more than 0.05 and less than or equal to 0.1 MPa;
the fifth stage: heating the high-temperature atmosphere furnace to 1350-1500 ℃ at the speed of 5-10 ℃/min; the atmosphere in the furnace is an oxidizing atmosphere, and the pressure in the furnace is more than 0.1 and less than or equal to 0.5 MPa;
the sixth stage: preserving the heat of the high-temperature atmosphere furnace for 30-180 min at 1350-1500 ℃, wherein the atmosphere in the furnace is air atmosphere;
step 2, preparation methods of aluminum-silicon-nickel alloy @ ceramic macrocapsule, aluminum-silicon-iron alloy @ ceramic macrocapsule and aluminum-silicon alloy @ ceramic macrocapsule
Placing the aluminum-silicon-nickel alloy ball into a ceramic spherical shell to obtain an aluminum-silicon-nickel alloy @ ceramic macrocapsule;
putting the ferro-aluminum-silicon alloy ball into a ceramic spherical shell to obtain the ferro-aluminum-silicon alloy @ ceramic macrocapsule;
placing the aluminum-silicon alloy ball into a ceramic spherical shell to obtain an aluminum-silicon alloy @ ceramic macrocapsule;
the diameter of the alloy ball is 2-18 mm, and the alloy ball is one of an aluminum-silicon-nickel alloy ball, an aluminum-silicon-iron alloy ball and an aluminum-silicon alloy ball; the aluminum-silicon-nickel alloy balls, the aluminum-silicon-iron alloy balls and the aluminum-silicon alloy balls are respectively made of corresponding aluminum-silicon-nickel alloy rods, aluminum-silicon-iron alloy rods and aluminum-silicon alloy rods;
step 3, preparation method of high-temperature phase-change heat storage refractory material
55-65 wt% of aluminum-silicon-nickel alloy @ ceramic macrocapsule is used as an aggregate, 25-35 wt% of aluminum-silicon-nickel alloy @ alumina microcapsule and 4-6 wt% of α -Al2O3Micro powder, 0.1-1 wt% of silicon micro powder and 4-6 wt% of calcium aluminate cement are used as matrixes, and the sum of aggregate and the matrixes is used as raw materials; uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing at 25-28 ℃ for 24-30 h with the relative air humidity of 75-80%, demolding, and drying at 110-300 ℃ for 24-36 h to prepare the high-temperature phase change heat storage refractory material;
the phase change temperature of the high-temperature phase change heat storage refractory material is 1150-1300 ℃;
step 4, preparation method of intermediate-temperature phase-change heat storage refractory material
55-65 wt% of ferro-silicon-aluminum alloy @ ceramic macrocapsule is used as aggregate, 25-35 wt% of ferro-silicon-aluminum alloy @ alumina microcapsule and 4-6 wt% of α -Al2O3Micro powder, 0.1-1 wt% of silicon micro powder and 4-6 wt% of calcium aluminate cement are used as matrixes, and the sum of aggregate and the matrixes is used as raw materials; uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting and molding, maintaining for 24-30 h at the temperature of 25-28 ℃ and the relative air humidity of 75-80%, demolding, and then maintaining at 110-EDrying for 24-36 h at 300 ℃ to prepare the intermediate-temperature phase-change heat-storage refractory material;
the phase change temperature of the medium-temperature phase change heat storage refractory material is 800-950 ℃;
step 5, preparation method of low-temperature phase-change heat storage refractory material
55-65 wt% of aluminum-silicon alloy @ ceramic macrocapsule is used as aggregate, 25-35 wt% of aluminum-silicon alloy @ alumina microcapsule and 4-6 wt% of α -Al2O3Micro powder, 0.1-1 wt% of silicon micro powder and 4-6 wt% of calcium aluminate cement are used as matrixes, and the sum of aggregate and the matrixes is used as raw materials; uniformly mixing the substrate and polycarboxylic acid accounting for 0.1-0.2 wt% of the raw materials to obtain a premixed substrate material; mixing the premixed matrix material and the aggregate, adding water accounting for 3-5 wt% of the raw materials, uniformly stirring, casting, curing at 25-28 ℃ for 24-30 h with the relative air humidity of 75-80%, demolding, and drying at 110-300 ℃ for 24-36 h to prepare the low-temperature phase change heat storage refractory material;
the phase change temperature of the low-temperature phase change heat storage refractory material is 500-650 ℃;
step 6, preparation method of batch-type operation high-temperature kiln near-zero heat loss refractory material lining body
The batch-type operation high-temperature kiln near-zero heat loss refractory material lining body sequentially comprises the following components from inside to outside along the thickness direction: working lining refractory material, permanent lining refractory material and heat insulation lining heat preservation material;
the working lining refractory material is positioned on a hot surface contacting a high-temperature medium in the kiln, and the thickness of the working lining refractory material is 150-250 mm;
the heat insulation lining and heat insulation material is a nano heat insulation plate, and the thickness of the heat insulation lining and heat insulation material is 5-20 mm;
the permanent lining refractory material is a phase change heat storage refractory material, and the phase change heat storage refractory material is composed of a high-temperature phase change heat storage refractory material, a medium-temperature phase change heat storage refractory material and a low-temperature phase change heat storage refractory material in sequence from inside to outside; wherein:
the thickness of the high-temperature phase-change heat-storage refractory material is 30-80 mm;
the thickness of the medium-temperature phase-change heat storage refractory material is 20-60 mm;
the thickness of the low-temperature phase-change heat-storage refractory material is 30-110 mm;
the intermittently operated high-temperature kiln is one of a ladle, a torpedo tank, a ladle, a shuttle kiln and a down-draft kiln, and the refractory lining body comprises a top, a bottom and a wall body.
2. The method for preparing a near-zero heat loss refractory lining for a batch-type operated high-temperature kiln according to claim 1, wherein the method for preparing the ceramic spherical shell comprises the following steps:
ball-milling 80-90 wt% of corundum fine powder, 5-15 wt% of mullite fine powder, 3-5 wt% of α -alumina powder micro powder and 1-3 wt% of silicon dioxide micro powder in a ball mill for 5-8 min to obtain mixed powder, adding 5-20 wt% of zirconium dioxide sol into the mixed powder, uniformly stirring to obtain mixed pug, molding the mixed pug by using an injection molding machine to obtain a hemispherical shell mud blank with threads, drying the hemispherical shell mud blank with threads at 110-180 ℃ for 24-36 h, heating to 1350-1650 ℃ at the speed of 3-5 ℃/min, and preserving heat for 2-4 h to obtain the ceramic hemispherical shell with threads;
the ceramic hemispherical shell with the threads is a ceramic hemispherical shell with internal threads and a ceramic hemispherical shell with external threads; the ceramic hemispherical shell with the internal thread and the ceramic hemispherical shell with the external thread are connected into a hollow sphere through the thread, and then the ceramic spherical shell is obtained;
the inner thread is arranged on the annular inner wall at the edge of the hemispherical ceramic shell with the inner thread, and the outer thread is arranged on the annular outer wall at the edge of the hemispherical ceramic shell with the outer thread; the ceramic hemispherical shell with the internal thread and the ceramic hemispherical shell with the external thread have the same outer diameter and wall thickness; the wall thickness is 0.6-2 mm, and the outer diameter is 3.5-24 mm; the nominal diameter of the internal thread and the external thread is 2.7-21 mm; al of the corundum fine powder2O3The content is more than or equal to 98 wt%; the grain size of the corundum fine powder is less than or equal to 15 mu m;
the mullite fine powder comprises the following components: al (Al)2O3The content is more than or equal to 70wt percent, and SiO is2The content is more than or equal to 22 wt%; the grain diameter of the mullite fine powder is less than or equal to 15 mu m;
the zirconium dioxide sol has a solid content of 30 wt% and a particle size of 20-50 nm.
3. The method for preparing a near-zero heat loss refractory lining for a batch-type operated high-temperature kiln according to claim 1, wherein the aluminum silicon nickel alloy rod comprises the following chemical components: 17-25 wt% of Al, 53-60 wt% of Si and 20-28 wt% of Ni; the aluminum-silicon-nickel alloy powder and the aluminum-silicon-nickel alloy rod have the same chemical components, and the particle size of the aluminum-silicon-nickel alloy powder is 13-250 mu m.
4. The method for producing a near-zero heat loss refractory lining for a batch-type operated high-temperature kiln according to claim 1, wherein the Al-Si-Fe alloy rod comprises the following chemical components: the Al content is 40-45 wt%, the Si content is 40-45 wt%, and the Fe content is 10-15 wt%; the aluminum-silicon-iron alloy powder and the aluminum-silicon-iron alloy rod have the same chemical composition, and the particle size of the aluminum-silicon-iron alloy powder is 13-250 mu m.
5. The method for preparing the near-zero heat loss refractory material lining of the intermittently operated high-temperature kiln according to claim 1, wherein the Si content of the aluminum-silicon alloy rod is 12-45 wt%; the silicon content of the aluminum-silicon alloy powder is the same as that of the aluminum-silicon alloy rod, and the particle size of the aluminum-silicon alloy powder is 13-250 mu m.
6. The method of making a near zero heat loss refractory lining for a batch operated high temperature furnace of claim 1, wherein said α -Al is present2O3Micronized Al2O3Content is more than or equal to 97wt percent, α -Al2O3The particle size of the micro powder is less than or equal to 8 mu m.
7. The method of claim 1, wherein the SiO of the fine silica powder is used as a refractory material in the form of a near zero heat loss refractory lining for batch-type high temperature furnaces2Content (wt.)>92 wt%; particle size of silica micropowder<1μm。
8. The method of making a near zero heat waste refractory lining for a batch operated high temperature kiln as claimed in claim 1, wherein the calcium aluminate cement has a chemical composition of: al (Al)2O350-60 wt% of SiO2Content (wt.)<8wt％，Fe2O3Content (wt.)<2.5 wt%; the grain diameter of the calcium aluminate cement is less than or equal to 10 mu m.
9. A near-zero heat loss refractory lining body of an intermittently operated high-temperature kiln, characterized in that the near-zero heat loss refractory lining body of the intermittently operated high-temperature kiln is the near-zero heat loss refractory lining body of the intermittently operated high-temperature kiln prepared by the method for preparing the near-zero heat loss refractory lining body of the intermittently operated high-temperature kiln according to any one of claims 1 to 8.
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