CN113526943A - High-durability rock wool and preparation method thereof - Google Patents

High-durability rock wool and preparation method thereof Download PDF

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Publication number
CN113526943A
CN113526943A CN202110867953.8A CN202110867953A CN113526943A CN 113526943 A CN113526943 A CN 113526943A CN 202110867953 A CN202110867953 A CN 202110867953A CN 113526943 A CN113526943 A CN 113526943A
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rock wool
durability
sol solution
parts
portions
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CN202110867953.8A
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Inventor
周文俊
王永林
谢春竹
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Tianchang Kangmeida New Insulation Material Co ltd
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Tianchang Kangmeida New Insulation Material Co ltd
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Priority to CN202110867953.8A priority Critical patent/CN113526943A/en
Publication of CN113526943A publication Critical patent/CN113526943A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00Compositions for artificial stone, not containing binders
    • C04B30/02Compositions for artificial stone, not containing binders containing fibrous materials
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/04Manufacture of glass fibres or filaments by using centrifugal force, e.g. spinning through radial orifices; Construction of the spinner cups therefor
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00Fibre or filament compositions
    • C03C13/06Mineral fibres, e.g. slag wool, mineral wool, rock wool
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/04Silica-rich materials; Silicates
    • C04B14/06Quartz; Sand
    • C04B14/064Silica aerogel
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38Fibrous materials; Whiskers
    • C04B14/383Whiskers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38Fibrous materials; Whiskers
    • C04B14/46Rock wool ; Ceramic or silicate fibres
    • C04B14/4643Silicates other than zircon
    • C04B14/4656Al-silicates, e.g. clay
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors

Abstract

The invention relates to the technical field of rock wool, in particular to high-durability rock wool and a preparation method thereof, wherein the rock wool comprises rock wool components and a modified sol solution, and the rock wool components comprise the following raw materials in parts by weight: 400 portions of basalt, 100 portions of dolomite, 200 portions of blast furnace slag and 80 portions to 100 portions of coke; according to the invention, the gel is formed on the surface of the rock wool component, so that the silicon dioxide aerogel is finally adhered to the surface of the rock wool component, the heat conductivity of the rock wool component is reduced, and the heat insulation property of the rock wool product is improved; because the surface of the silicon dioxide aerogel has hydrophilic groups, rock wool components are easy to absorb moisture, the heat conductivity is increased, and the heat preservation effect is reduced.

Description

High-durability rock wool and preparation method thereof
Technical Field
The invention relates to the technical field of rock wool, in particular to high-durability rock wool and a preparation method thereof.
Background
The existing commonly used wall heat-insulating materials are mainly divided into inorganic materials and organic materials, the organic materials are light in weight and good in heat-insulating and heat-insulating effects, but the most important defects of the materials are poor in fire safety and easy to burn, and the materials are large in smoke and toxicity during burning and are not as good as the inorganic heat-insulating materials in use safety. The inorganic heat-insulating material has good fireproof performance and no toxicity, and the application range is wider and wider.
The rock wool material is one of inorganic heat-insulating materials, is widely applied to building outer walls, and plays roles in heat preservation, heat insulation, sound absorption and noise reduction. Rock wool products in the prior art have high heat conductivity and general heat insulation. Therefore, we propose a high durability rock wool and a preparation method thereof to solve the above problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides high-durability rock wool and a preparation method thereof so as to overcome the problems in the background art.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme: the high-durability rock wool comprises rock wool components and a modified sol solution, wherein the rock wool components comprise the following raw materials in parts by weight: 400 portions of basalt, 100 portions of dolomite, 200 portions of blast furnace slag and 80 portions to 100 portions of coke.
Preferably, the rock wool component comprises the following raw materials in parts by weight: 350 parts of basalt, 150 parts of dolomite, 110 parts of blast furnace slag and 90 parts of coke.
Preferably, the preparation method of the modified sol solution is as follows: s1: putting tetraethoxysilane, deionized water and absolute ethyl alcohol into a reactor, uniformly stirring, slowly adding oxalic acid into the reactor, adjusting the pH value to 1-3, uniformly stirring, and reacting at 45-55 ℃ for 40-50min to obtain a sol solution; s2: adding potassium hexatitanate crystal whiskers into the sol solution, and performing ultrasonic dispersion to obtain a modified sol solution.
Preferably, the molar ratio of the ethyl orthosilicate to the deionized water to the absolute ethyl alcohol is (1-1.5): (3-4): (6-8).
Preferably, the concentration of the oxalic acid is 0.1 mol/L.
Preferably, the potassium hexatitanate whiskers account for 10-12% of the total mass of the sol solution.
The invention also provides a preparation method of the high-durability rock wool, which comprises the following steps:
(1) crushing basalt, dolomite, blast furnace slag and coke, and then putting the crushed basalt, dolomite, blast furnace slag and coke into a cupola to be melted at 1500-;
(2) centrifugally blowing the molten mass into fibers, spraying phenolic resin binder on the fibers, and then carrying out cotton collection, superposition, pressurized pleating and high-temperature pressurized shaping in a curing furnace to obtain rock wool components;
(3) putting the rock wool component into the modified sol solution, adding ammonia water into the modified sol solution, adjusting the pH value to 7-8, and performing polycondensation reaction to form gel on the surface of the rock wool component;
(4) soaking the product obtained in the step (3) in absolute ethyl alcohol, aging at normal temperature for 48h, and replacing the surface solvent with n-hexane for 24 h;
(5) putting the product obtained in the step (4) into methanol steam, controlling the temperature of the methanol steam to be 220-240 ℃, and carrying out oxidation treatment for 12-15 h;
(6) and (5) drying the product obtained in the step (5) to obtain the high-durability rock wool.
Preferably, in the step (3), the concentration of the ammonia water is 1 mol/L.
The invention has the beneficial effects that:
according to the invention, the gel is formed on the surface of the rock wool component, so that the silicon dioxide aerogel is finally adhered to the surface of the rock wool component, the heat conductivity of the rock wool component is reduced, and the heat insulation property of the rock wool product is improved; because the surface of the silicon dioxide aerogel has hydrophilic groups, rock wool components are easy to absorb moisture, the heat conductivity is increased, and the heat preservation effect is reduced3The hydrophobicity of the silicon dioxide aerogel is increased, and the heat insulation performance of the rock wool product is ensured;
according to the invention, the potassium hexatitanate whisker is added, has a unique tunnel-shaped structure, has structural chemical inertness and unique heat insulation performance, and is mixed and dispersed in the silica aerogel, so that the wear resistance of the silica aerogel is enhanced, the infrared radiation resistance of the silica aerogel is also improved, the heat insulation of the silica aerogel is further enhanced, and the heat insulation of rock wool products is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-durability rock wool comprises rock wool components and a modified sol solution, wherein the rock wool components comprise the following raw materials in parts by weight: 300 parts of basalt, 100 parts of dolomite, 100 parts of blast furnace slag and 80 parts of coke.
The preparation method of the modified sol solution is as follows, S1: putting ethyl orthosilicate, deionized water and absolute ethyl alcohol into a reactor, uniformly stirring, slowly adding oxalic acid into the reactor, adjusting the pH to 2, uniformly stirring, and reacting at 45 ℃ for 40min to obtain a sol solution; s2: adding potassium hexatitanate crystal whiskers into the sol solution, and performing ultrasonic dispersion to obtain a modified sol solution.
The molar ratio of the ethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1: 3: 7; the concentration of oxalic acid is 0.1 mol/L; the potassium hexatitanate whisker accounts for 10 percent of the total mass of the sol solution.
The preparation method of the high-durability rock wool comprises the following steps:
(1) crushing basalt, dolomite, blast furnace slag and coke, and then putting the crushed basalt, dolomite, blast furnace slag and coke into a cupola furnace to melt at 1600 ℃ to obtain a molten mass;
(2) centrifugally blowing the molten mass into fibers, spraying phenolic resin binder on the fibers, and then carrying out cotton collection, superposition, pressurized pleating and high-temperature pressurized shaping in a curing furnace to obtain rock wool components;
(3) putting the rock wool component into the modified sol solution, adding 1mol/L ammonia water into the modified sol solution, adjusting the pH value to 7, and performing polycondensation reaction to form gel on the surface of the rock wool component;
(4) soaking the product obtained in the step (3) in absolute ethyl alcohol, aging at normal temperature for 48h, and replacing the surface solvent with n-hexane for 24 h;
(5) putting the product obtained in the step (4) into methanol steam, controlling the temperature of the methanol steam to be 220 ℃, and carrying out oxidation treatment for 12 h;
(6) and (5) drying the product obtained in the step (5) to obtain the high-durability rock wool.
Example 2
The high-durability rock wool comprises rock wool components and a modified sol solution, wherein the rock wool components comprise the following raw materials in parts by weight: 350 parts of basalt, 150 parts of dolomite, 110 parts of blast furnace slag and 90 parts of coke.
The preparation method of the modified sol solution is as follows, S1: putting ethyl orthosilicate, deionized water and absolute ethyl alcohol into a reactor, uniformly stirring, slowly adding oxalic acid into the reactor, adjusting the pH to 2, uniformly stirring, and reacting at 50 ℃ for 45min to obtain a sol solution; s2: adding potassium hexatitanate crystal whiskers into the sol solution, and performing ultrasonic dispersion to obtain a modified sol solution.
The molar ratio of the ethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1: 3: 7; the concentration of oxalic acid is 0.1 mol/L; the potassium hexatitanate whisker accounts for 10 percent of the total mass of the sol solution.
The preparation method of the high-durability rock wool comprises the following steps:
(1) crushing basalt, dolomite, blast furnace slag and coke, and then putting the crushed basalt, dolomite, blast furnace slag and coke into a cupola furnace to melt at 1600 ℃ to obtain a molten mass;
(2) centrifugally blowing the molten mass into fibers, spraying phenolic resin binder on the fibers, and then carrying out cotton collection, superposition, pressurized pleating and high-temperature pressurized shaping in a curing furnace to obtain rock wool components;
(3) putting the rock wool component into the modified sol solution, adding 1mol/L ammonia water into the modified sol solution, adjusting the pH value to 7, and performing polycondensation reaction to form gel on the surface of the rock wool component;
(4) soaking the product obtained in the step (3) in absolute ethyl alcohol, aging at normal temperature for 48h, and replacing the surface solvent with n-hexane for 24 h;
(5) putting the product obtained in the step (4) into methanol steam, controlling the temperature of the methanol steam to be 230 ℃, and carrying out oxidation treatment for 13 h;
(6) and (5) drying the product obtained in the step (5) to obtain the high-durability rock wool.
Example 3
The high-durability rock wool comprises rock wool components and a modified sol solution, wherein the rock wool components comprise the following raw materials in parts by weight: 380 parts of basalt, 160 parts of dolomite, 120 parts of blast furnace slag and 95 parts of coke.
The preparation method of the modified sol solution is as follows, S1: putting ethyl orthosilicate, deionized water and absolute ethyl alcohol into a reactor, uniformly stirring, slowly adding oxalic acid into the reactor, adjusting the pH to 2, uniformly stirring, and reacting at 50 ℃ for 45min to obtain a sol solution; s2: adding potassium hexatitanate crystal whiskers into the sol solution, and performing ultrasonic dispersion to obtain a modified sol solution.
The molar ratio of the ethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1: 3: 7; the concentration of oxalic acid is 0.1 mol/L; the potassium hexatitanate whisker accounts for 10 percent of the total mass of the sol solution.
The preparation method of the high-durability rock wool comprises the following steps:
(1) crushing basalt, dolomite, blast furnace slag and coke, and then putting the crushed basalt, dolomite, blast furnace slag and coke into a cupola furnace to melt at 1600 ℃ to obtain a molten mass;
(2) centrifugally blowing the molten mass into fibers, spraying phenolic resin binder on the fibers, and then carrying out cotton collection, superposition, pressurized pleating and high-temperature pressurized shaping in a curing furnace to obtain rock wool components;
(3) putting the rock wool component into the modified sol solution, adding 1mol/L ammonia water into the modified sol solution, adjusting the pH value to 7, and performing polycondensation reaction to form gel on the surface of the rock wool component;
(4) soaking the product obtained in the step (3) in absolute ethyl alcohol, aging at normal temperature for 48h, and replacing the surface solvent with n-hexane for 24 h;
(5) putting the product obtained in the step (4) into methanol steam, controlling the temperature of the methanol steam to be 230 ℃, and carrying out oxidation treatment for 13 h;
(6) and (5) drying the product obtained in the step (5) to obtain the high-durability rock wool.
Example 4
The high-durability rock wool comprises rock wool components and a modified sol solution, wherein the rock wool components comprise the following raw materials in parts by weight: 400 parts of basalt, 200 parts of dolomite, 120 parts of blast furnace slag and 100 parts of coke.
The preparation method of the modified sol solution is as follows, S1: putting ethyl orthosilicate, deionized water and absolute ethyl alcohol into a reactor, uniformly stirring, slowly adding oxalic acid into the reactor, adjusting the pH value to 3, uniformly stirring, and reacting at 55 ℃ for 50min to obtain a sol solution; s2: adding potassium hexatitanate crystal whiskers into the sol solution, and performing ultrasonic dispersion to obtain a modified sol solution.
The molar ratio of the ethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1.5: 4: 8; the concentration of oxalic acid is 0.1 mol/L; the potassium hexatitanate whisker accounts for 12 percent of the total mass of the sol solution.
The preparation method of the high-durability rock wool comprises the following steps:
(1) crushing basalt, dolomite, blast furnace slag and coke, and then putting the crushed basalt, dolomite, blast furnace slag and coke into a cupola furnace to melt at 1750 ℃ to obtain a molten mass;
(2) centrifugally blowing the molten mass into fibers, spraying phenolic resin binder on the fibers, and then carrying out cotton collection, superposition, pressurized pleating and high-temperature pressurized shaping in a curing furnace to obtain rock wool components;
(3) putting the rock wool component into the modified sol solution, adding 1mol/L ammonia water into the modified sol solution, adjusting the pH value to 8, and performing polycondensation reaction to form gel on the surface of the rock wool component;
(4) soaking the product obtained in the step (3) in absolute ethyl alcohol, aging at normal temperature for 48h, and replacing the surface solvent with n-hexane for 24 h;
(5) putting the product obtained in the step (4) into methanol steam, controlling the temperature of the methanol steam to be 240 ℃, and carrying out oxidation treatment for 15 h;
(6) and (5) drying the product obtained in the step (5) to obtain the high-durability rock wool.
Performance detection
1. The test method comprises the following steps: the products of examples 1-4 were tested for thermal conductivity according to GB/T10294-2008. The heat conductivity coefficient of the common rock wool product is 0.04W/(m.k), and the specific detection result is shown in Table 1.
TABLE 1 thermal conductivity
Group of Thermal conductivity, W/(m.k)
Example 1 0.0315
Example 2 0.0323
Example 3 0.0317
Example 1 0.0336
2. The test method comprises the following steps: the contact angles of the products of examples 1 to 4 with pure water were measured at room temperature using a Sl200A contact angle tester. Specific detection results are shown in table 2.
TABLE 2 hydrophobic Properties
Group of Surface contact angle
Example 1 136.8
Example 2 138.1
Example 3 136.3
Example 1 135.6
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. The high-durability rock wool is characterized by comprising rock wool components and a modified sol solution, wherein the rock wool components comprise the following raw materials in parts by weight: 400 portions of basalt, 100 portions of dolomite, 200 portions of blast furnace slag and 80 portions to 100 portions of coke.
2. The high-durability rock wool according to claim 1 wherein said rock wool module comprises the following raw materials in parts by weight: 350 parts of basalt, 150 parts of dolomite, 110 parts of blast furnace slag and 90 parts of coke.
3. The high-durability rock wool according to claim 1, wherein the modified sol solution is prepared by the following steps:
s1: putting tetraethoxysilane, deionized water and absolute ethyl alcohol into a reactor, uniformly stirring, slowly adding oxalic acid into the reactor, adjusting the pH value to 1-3, uniformly stirring, and reacting at 45-55 ℃ for 40-50min to obtain a sol solution;
s2: adding potassium hexatitanate crystal whiskers into the sol solution, and performing ultrasonic dispersion to obtain a modified sol solution.
4. The high-durability rock wool as claimed in claim 3, wherein the mole ratio of said tetraethoxysilane to said deionized water to said absolute ethyl alcohol is (1-1.5): (3-4): (6-8).
5. The high-durability rock wool as claimed in claim 3, wherein said oxalic acid concentration is 0.1 mol/L.
6. The high-durability rock wool according to claim 3, wherein said potassium hexatitanate whiskers account for 10-12% of the total mass of the sol solution.
7. The method for preparing the high-durability rock wool according to any one of claims 1 to 6, which is characterized by comprising the following steps:
(1) crushing basalt, dolomite, blast furnace slag and coke, and then putting the crushed basalt, dolomite, blast furnace slag and coke into a cupola to be melted at 1500-;
(2) centrifugally blowing the molten mass into fibers, spraying phenolic resin binder on the fibers, and then carrying out cotton collection, superposition, pressurized pleating and high-temperature pressurized shaping in a curing furnace to obtain rock wool components;
(3) putting the rock wool component into the modified sol solution, adding ammonia water into the modified sol solution, adjusting the pH value to 7-8, and performing polycondensation reaction to form gel on the surface of the rock wool component;
(4) soaking the product obtained in the step (3) in absolute ethyl alcohol, aging at normal temperature for 48h, and replacing the surface solvent with n-hexane for 24 h;
(5) putting the product obtained in the step (4) into methanol steam, controlling the temperature of the methanol steam to be 220-240 ℃, and carrying out oxidation treatment for 12-15 h;
(6) and (5) drying the product obtained in the step (5) to obtain the high-durability rock wool.
8. The method for preparing high-durability rock wool according to claim 7, wherein in the step (3), the concentration of the ammonia water is 1 mol/L.
CN202110867953.8A 2021-07-30 2021-07-30 High-durability rock wool and preparation method thereof Pending CN113526943A (en)

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CN115140943A (en) * 2022-06-30 2022-10-04 北京中环鑫汇科技有限公司 Method for producing rock wool by utilizing solid wastes of iron and steel plant
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Application publication date: 20211022

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