CN110776266B - Preparation method of building material with electromagnetic wave absorption function - Google Patents

Preparation method of building material with electromagnetic wave absorption function Download PDF

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CN110776266B
CN110776266B CN201911081629.2A CN201911081629A CN110776266B CN 110776266 B CN110776266 B CN 110776266B CN 201911081629 A CN201911081629 A CN 201911081629A CN 110776266 B CN110776266 B CN 110776266B
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cobalt
zinc
manganese
copper
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CN110776266A (en
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刘兵兵
韩桂洪
黄艳芳
苏胜鹏
杨淑珍
王文娟
薛毓斌
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Zhengzhou University
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • 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
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
    • C04B7/42—Active ingredients added before, or during, the burning process
    • C04B7/428—Organic materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

Abstract

The invention discloses a method for preparing a building material with an electromagnetic wave absorption function, which comprises the steps of finely grinding, uniformly mixing, preheating, roasting, cooling and finely grinding clay, a manganese-containing material, an iron-containing material, a zinc-containing material, a copper-containing material, a cobalt-containing material, a calcium material, a silicon material and a binder to obtain the cement building material with the electromagnetic wave absorption function.

Description

Preparation method of building material with electromagnetic wave absorption function
Technical Field
The invention relates to a preparation method of a building material with an electromagnetic wave absorption function, in particular to a method for preparing a cement building material with the electromagnetic wave absorption function in one step by carrying out organic fusion grafting on low-grade minerals and waste residue raw materials and a traditional cement production process.
Background
With the rapid development of modern electronic science and technology, electronic equipment is high-frequency and digital, electromagnetic radiation and the like create wealth for human beings, and meanwhile, the equipment, a system and the ecological environment are more and more seriously damaged, so that the electromagnetic radiation is internationally recognized as the fourth public nuisance following atmospheric pollution, water quality pollution and noise pollution. At an airport, airplane flights are mistakenly clicked because the airplane cannot take off due to electromagnetic wave interference; in hospitals, mobile phones often interfere with the normal operation of various electronic medical instruments. In order to prevent external electromagnetic interference and leakage of electromagnetic signals, reduce the damage of electromagnetic waves to human bodies and the detection capability of electromagnetic waves to buildings, purify electromagnetic radiation, improve the electromagnetic environment of building spaces, and eliminate electromagnetic pollution, electromagnetic protection of buildings is required. Therefore, the wave-absorbing material, which is a material capable of resisting and weakening electromagnetic wave radiation, is a major subject of material science to be found for treating electromagnetic pollution.
The tall buildings in the city stand in forest, and the reflected electromagnetic waves of the tall buildings can cause double images. The wave-absorbing material is applied to building materials, so that the problem can be solved easily. The microwave anechoic chamber made of the wave-absorbing material can be widely applied to the fields of radar, communication and aerospace. In addition, the wave-absorbing material has wide application space in the aspects of improving the compatibility of airborne and airborne radar equipment, improving the performance of the whole machine and the like.
By a wave absorbing material is meant a material that absorbs the energy of the electromagnetic waves incident on its surface. In engineering application, the wave-absorbing material is required to have high absorption rate to electromagnetic waves in a wider frequency band, and also required to have the properties of temperature resistance, moisture resistance, corrosion resistance and the like. The cement material in China has abundant resources, low energy consumption of products, strong adaptability and good durability, and is a building material which is widely applied to bearing and maintaining the shape of buildings. However, pure cement does not have a shielding and absorbing effect of electromagnetic waves, and is generally filled with an electromagnetic shielding material so that radiation and leakage of electromagnetic waves can be effectively suppressed. Common wave-absorbing media in cement include graphite, ferrite, and the like.
The patent document "cement base material wave-absorbing building material (CN 201210526460.9)" provides a cement-based wave-absorbing building material which takes closed-cell expanded perlite as a cement matrix and graphite micropowder as a wave-absorbing medium. The technical scheme takes graphite micropowder with poor wettability and small density as a wave-absorbing medium, and has the defects of difficult wetting, easy dust raising and easy segregation during use. The document "research on wave absorption performance of manganese-zinc ferrite cement-based composite material, volume 10, phase 4, the building materials bulletin" discloses that manganese-zinc ferrite is obtained by using iron oxide, zinc oxide and manganese carbonate as raw materials through ball milling and calcination, and then is compounded with cement to prepare the cement-based composite wave absorption material. The technology is that pure substances (manganese oxide, iron oxide and the like) are firstly prepared into a wave-absorbing material with good performance, then the wave-absorbing material is finely ground to a certain granularity and is added into a cement building material to prepare the cement-based composite wave-absorbing material with a certain wave-absorbing performance. However, the process is complex, two single and parallel processes are needed to prepare the wave-absorbing material and the cement respectively, and then the cement-based composite wave-absorbing material is prepared by mixing, so that the process is complex, the equipment investment cost is high, the raw material cost is high, and the industrial large-scale production is not facilitated.
Disclosure of Invention
Aiming at the defects that two high-temperature processes are needed in the preparation process of the cement-based composite wave-absorbing material with wave-absorbing performance, the cost of raw materials is high and the like at present, the invention aims to provide a method for preparing a building material with an electromagnetic wave-absorbing function by adopting low-quality minerals, waste residues and other cheap raw materials to perform one-step high-temperature roasting, and the method can simultaneously realize high-value utilization of low-value minerals and solid waste resources and preparation integration of high-performance building materials and has higher economic value.
In order to achieve the technical purpose, the invention provides a method for preparing a building material with an electromagnetic wave absorption function, which comprises the steps of finely grinding clay, a manganese-containing material, an iron-containing material, a zinc-containing material, a copper-containing material, a cobalt-containing material, a calcium material, a siliceous material and a binder, uniformly mixing, preheating at 900-1050 ℃ and roasting at 1250-1350 ℃ in sequence, cooling and finely grinding the roasted material to obtain the building material;
wherein the ingredients of the clay, the manganese-containing material, the iron-containing material, the zinc-containing material, the copper-containing material, the cobalt-containing material, the calcareous material, the siliceous material and the binder satisfy the following relations: the molar ratio of (Mn + Zn + Cu + Co)/Fe is 1.0-2.5, and the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) is not less than 0.2; the proportion of the calcareous material and the siliceous material meets the CaO/SiO ratio in the mixed raw materials2The molar ratio of (A) to (B) is between 1.9 and 3.0; and the total mass percentage of the oxides of manganese, iron, zinc, cobalt and copper in the mixed raw materials is 10-30%.
The technical scheme of the invention adopts low-grade manganese, zinc, iron, cobalt and copper minerals or solid waste resources as raw materials, regulates and controls chemical components in the mixture and controls roasting conditions, and generates a spinel structure composite ferrite phase with good wave-absorbing performance and simultaneously generates main phases required by cement by using oxides of calcium, silicon, aluminum and the like in the mixture. The synchronous in-situ generation and compounding of the phases of the composite ferrite and the calcium silicate in the roasting process are realized, the phases of the composite ferrite and the calcium silicate are more uniformly distributed in cement clinker, the building material is endowed with better wave-absorbing performance, and compared with the prior art, the procedure that two high-temperature procedures are respectively used for preparing the composite ferrite and the cement and are required to be uniformly mixed by force can be omitted.
The ferrite wave-absorbing material with multiple elements in the building material prepared by the invention has the characteristics of high absorption frequency band, high absorption rate, thin matching thickness and the like, and utilizes the ferrite with high magnetic conductivity to guide electromagnetic waves, absorbs a large amount of radiation energy of the electromagnetic waves through resonance, and converts the energy of the electromagnetic waves into heat energy through coupling, thereby achieving the purpose of eliminating electromagnetic interference. Compared with the traditional binary manganese zinc ferrite, the multi-element ferrite wave-absorbing material has better wave-absorbing performance.
In the preferred scheme, clay, manganese-containing materials, iron-containing materials, zinc-containing materials, copper-containing materials, cobalt-containing materials, calcium materials and siliceous materials are finely ground until the mass percentage content of the granularity which is less than 400 meshes is not less than 99 percent and the specific surface area is not less than 3000cm2(ii) in terms of/g. In the preferable range of particle size and specific surface area, the mass transfer efficiency of the high-temperature solid-phase reaction is improved.
In a preferred embodiment, the clay comprises at least one of kaolin and illite.
Preferably, the manganese-containing material comprises at least one of pyrolusite, manganese carbonate ore and ferromanganese ore.
In a preferred embodiment, the iron-containing material includes at least one of magnetite, hematite, limonite, goethite, siderite, and rolled steel sheet.
Preferably, the zinc-containing material comprises at least one of zinc-containing minerals, zinc calcine and purified cobalt slag.
Preferably, the copper-containing material comprises at least one of copper concentrate and copper slag.
Preferably, the cobalt-containing material comprises at least one of cobalt concentrate and cobalt-containing waste.
In a preferred scheme, the calcareous material comprises at least one of limestone and quicklime.
Preferably, the siliceous material provides primarily a silica component, and ideally, a source that provides silica is suitable for the present invention, preferably inexpensive silica.
In a preferred scheme, the binder is a common sintering additive, and the lignite humic acid is preferred in the invention.
According to the technical scheme, the clay, the manganese-containing material, the iron-containing material, the zinc-containing material, the copper-containing material, the cobalt-containing material, the calcium material and the siliceous material are common minerals and solid waste residues in the prior art, and have the characteristics of wide sources and low cost.
In a preferable scheme, the preheating time is 30 min-120 min.
In a preferable scheme, the roasting time is 60 min-180 min.
In a preferred embodiment, both preheating and baking are carried out in an air atmosphere.
In the preferred scheme, the roasted material is finely ground until the mass percentage content of the particle size which is less than 500 meshes is not less than 99 percent and the specific surface area is not less than 4000cm2/g。
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
the technical scheme of the invention takes low-grade manganese, zinc, iron, cobalt and copper minerals or solid waste resources as raw materials to prepare the building material with high utilization value and electromagnetic wave absorption function, thereby really realizing resource utilization.
The technical scheme of the invention realizes one-step high-temperature solid-phase reaction to obtain the building material with the electromagnetic wave absorption function by reasonably matching components and controlling roasting conditions, simplifies the process steps compared with the prior art, and the generation and compounding of the multi-element composite ferrite and the portland cement with the gel function are synchronously generated in situ in the roasting process, so that the two are more uniformly distributed, and the process of forcibly and uniformly mixing the composite ferrite and the cement prepared by the traditional two-step high-temperature process respectively can be omitted.
The building material in the technical scheme of the invention forms the multi-component composite ferrite, and compared with the traditional binary manganese zinc ferrite, the microwave absorbing property is better.
The technical scheme of the invention has simple process and low raw material cost, and is more favorable for industrial production.
The ground non-moving military target built by the high-performance building material has the function of interfering radar detection, can meet the requirements of human living and working environments on electromagnetic ferry radiation protection, and has very important significance on the development of special cement industry.
Drawings
Fig. 1 is a graph comparing the electromagnetic wave reflectance of the samples obtained in example 1 and comparative example 1.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Comparative example 1
Manganese-containing materials, zinc-containing materials, cobalt-containing materials and copper-containing materials are not added.
Taking kaolin, quicklime and silica as raw materials to prepare the materials, controlling the content of the humic acid binder of the lignite to be 0.35 percent and controlling CaO/SiO in the mixture2The molar ratio of (A) is 2.5, the mass percentage content of the mixture ground to a particle size less than 400 meshes is 100 percent, and the specific surface area is 3000cm2(ii) in terms of/g. Preheating the mixture at 900 deg.C for 120min, calcining at 1350 deg.C for 60min, cooling in air to room temperature, and fine grinding to particle sizeThe mass percentage content of the particle fraction satisfying-500 meshes is 100%, and the specific surface area is 4200cm2And/g, obtaining the cement building material. The building material has the reflectivity of only-2.5 dB to electromagnetic waves within the frequency range of 2-18 GHz.
Comparative example 2
The formulation chemistry in this comparative example is not within the preferred ranges.
The method comprises the following steps of preparing raw materials of illite, limestone, silica, manganese oxide ore containing 25% of manganese, mill scale containing 68% of iron, zinc calcine containing 58% of zinc, copper slag containing 1.6% of copper and cobalt concentrate containing 10% of cobalt, wherein the usage amount of a lignite humic acid binder is 0.5%, the molar ratio of (Mn + Zn + Cu + Co)/Fe in a mixture is controlled to be 0.5, and the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) is 0.1; the proportion of the calcareous and siliceous materials is that CaO/SiO in the mixed raw materials is satisfied2The molar ratio of the manganese to the iron to the zinc is 3.0, and the total mass percentage of the oxides of the manganese, the iron, the zinc, the cobalt and the copper in the mixture is 20 percent; the mixture is finely ground to the mass percentage content of less than 400 meshes of particle size of 100 percent, and the specific surface area is 3100cm2(ii) in terms of/g. Preheating the mixture at 1000 deg.C for 90min, calcining at 1300 deg.C for 120min, cooling in air to room temperature, and grinding to obtain powder with granularity less than 500 meshes, mass percentage content of 100%, and specific surface area of 4480cm2And/g, obtaining the building material with the electromagnetic wave absorption function. The building material has the reflectivity of only-3.6 dB to electromagnetic waves within the frequency range of 2-18 GHz.
Comparative example 3
In the comparative example, the mass percentage of the total oxide of manganese, iron, zinc, cobalt and copper in the mixture is not in the preferred range.
The method comprises the following steps of preparing raw materials of kaolinite, limestone, silica, manganese oxide ore containing 25% of manganese, rolling steel sheet containing 70% of iron, zinc calcine containing 58% of zinc, copper slag containing 1.5% of copper and cobalt concentrate containing 16% of cobalt, wherein the consumption of a lignite humic acid binder is 0.45%, the molar ratio of (Mn + Zn + Cu + Co)/Fe in a mixture is controlled to be 2.0, and the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) is 0.4; the proportion of the calcareous and siliceous materials is that CaO/SiO in the mixed raw materials is satisfied2In a molar ratio of 3.0, wherein manganese, iron,The total mass percentage of the oxides of zinc, cobalt and copper in the mixture is only 5%; the mixture is finely ground to the mass percentage content of less than 400 meshes of particle size of 100 percent, and the specific surface area is 3250cm2(ii) in terms of/g. Preheating the mixture at 1000 deg.C for 90min, calcining at 1300 deg.C for 120min, cooling in air to room temperature, and grinding to obtain powder with particle size of less than 500 meshes, mass percentage content of 100%, and specific surface area of 4260cm2And/g, obtaining the building material with the electromagnetic wave absorption function. The building material has the reflectivity of only-4.6 dB to electromagnetic waves within the frequency range of 2-18 GHz.
Example 1
Taking kaolin, quicklime, silica, manganese oxide ore containing 25% of manganese, steel rolling sheet containing 68% of iron, zinc calcine containing 52% of zinc, copper slag containing 1.6% of copper and cobalt concentrate containing 8% of cobalt as raw materials to prepare materials, wherein the dosage of the lignite humic acid binder is 0.5%, the molar ratio of (Mn + Zn + Cu + Co)/Fe in the mixture is controlled to be 2.5, and the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) is 0.2; the proportion of the calcareous and siliceous materials is that CaO/SiO in the mixed raw materials is satisfied2The molar ratio of the manganese to the iron to the zinc is 3.0, and the total mass percentage of the oxides of the manganese, the iron, the zinc, the cobalt and the copper in the mixture is 30 percent; the mixture is finely ground to the mass percentage content of less than 400 meshes of particle size of 100 percent, and the specific surface area is 3100cm2(ii) in terms of/g. Preheating the mixture at 900 deg.C for 120min, calcining at 1350 deg.C for 60min, cooling in air to room temperature, and grinding to obtain particles with a size of less than 500 meshes, a mass percentage content of 100%, and a specific surface area of 4850cm2And/g, obtaining the building material with the electromagnetic wave absorption function. The building material has a reflectivity of-9.4 dB to electromagnetic waves within a frequency range of 2-18 GHz.
Example 2
Taking kaolin, illite, limestone, silica, manganese carbonate ore containing 20% of manganese, magnetite containing 63% of iron, purified cobalt slag containing 50% of zinc, copper slag containing 2.1% of copper and cobalt concentrate containing 6% of cobalt as raw materials to prepare materials, wherein the dosage of the lignite humic acid binder is 0.4%, the molar ratio of (Mn + Zn + Cu + Co)/Fe in the mixture is controlled to be 1.0, and the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) is 0.5; calcareous and siliceous materialThe proportion of the materials should meet the CaO/SiO ratio in the mixed raw materials2The molar ratio of the manganese to the iron to the zinc is 1.9, and the total mass percentage of the oxides of the manganese, the iron, the zinc, the cobalt and the copper in the mixture is 10 percent; the mixture is finely ground to the mass percentage content of less than 400 meshes of particle size of 100 percent, and the specific surface area is 3200cm2(ii) in terms of/g. Roasting the mixture at 1050 deg.C for 30min and 1250 deg.C for 180min, respectively, cooling to room temperature in air, and grinding to obtain particles with a size of less than 500 meshes, a mass percentage content of 100%, and a specific surface area of 4400cm2And/g, obtaining the building material with the electromagnetic wave absorption function. The building material has a reflectivity of-9.2 dB to electromagnetic waves within a frequency range of 2-18 GHz.
Example 3
Taking kaolin, illite, limestone, silica, 18% manganese-containing iron-manganese ore, 67% iron-containing hematite, 45% zinc-containing purified cobalt slag, 1.3% copper-containing copper slag and 4.8% cobalt-containing concentrate as raw materials to prepare materials, controlling the dosage of a lignite humic acid binder to be 0.5%, controlling the molar ratio of (Mn + Zn + Cu + Co)/Fe in the mixture to be 2.0, and controlling the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) to be 0.4; the proportion of the calcareous and siliceous materials is that CaO/SiO in the mixed raw materials is satisfied2The molar ratio of (A) is 2.2, and the mass percentage of the total oxides of manganese, iron, zinc, cobalt and copper in the mixture is 15%; the mixture is finely ground to the mass percentage content of less than 400 meshes of particle size of 100 percent, and the specific surface area is 3400cm2(ii) in terms of/g. Roasting the mixture at 1050 deg.C for 30min and 1300 deg.C for 100min, respectively, cooling to room temperature in air, and grinding to obtain powder with particle size of less than 500 meshes, mass percentage content of 100%, and specific surface area of 4500cm2And/g, obtaining the building material with the electromagnetic wave absorption function. The building material has a reflectivity of-9.4 dB to electromagnetic waves within a frequency range of 2-18 GHz.

Claims (4)

1. A preparation method of a building material with an electromagnetic wave absorption function is characterized by comprising the following steps: finely grinding clay, a manganese-containing material, an iron-containing material, a zinc-containing material, a copper-containing material, a cobalt-containing material, a calcium material, a silicon material and a binder, uniformly mixing, sequentially preheating at 900-1050 ℃ for 30-120 min and roasting at 1250-1350 ℃ for 60-180 min, wherein the preheating and the roasting are carried out in an air atmosphere, and cooling and finely grinding the roasted material to obtain the material;
wherein the ingredients of the clay, the manganese-containing material, the iron-containing material, the zinc-containing material, the copper-containing material, the cobalt-containing material, the calcareous material, the siliceous material and the binder satisfy the following relations:
the molar ratio of (Mn + Zn + Cu + Co)/Fe is 1.0-2.5, and the molar ratio of (Zn + Cu + Co)/(Mn + Zn + Co + Cu) is not less than 0.2; the proportion of the calcareous material and the siliceous material meets the CaO/SiO ratio in the mixed raw materials2The molar ratio of (A) to (B) is between 1.9 and 3.0; and the total mass percentage of the oxides of manganese, iron, zinc, cobalt and copper in the mixed raw materials is 10-30%.
2. The method for preparing a building material having an electromagnetic wave absorption function according to claim 1, wherein: the clay, the manganese-containing material, the iron-containing material, the zinc-containing material, the copper-containing material, the cobalt-containing material, the calcium material and the silicon material are all finely ground until the mass percentage content of the granularity which is less than 400 meshes is not less than 99 percent, and the specific surface area is not less than 3000cm2/g。
3. The method for preparing a building material having an electromagnetic wave absorption function according to claim 1, wherein:
the clay comprises at least one of kaolin and illite;
the manganese-containing material comprises at least one of pyrolusite, manganese carbonate ore and ferromanganese ore;
the iron-containing material comprises at least one of magnetite, hematite, limonite, goethite, siderite and rolled steel sheet;
the zinc-containing material comprises at least one of zinc-containing minerals, zinc calcine and purified cobalt slag;
the copper-containing material comprises at least one of copper concentrate and copper slag;
the cobalt-containing material comprises at least one of cobalt concentrate and cobalt-containing waste;
the calcareous material comprises at least one of limestone and quicklime;
the siliceous material is silica;
the binder is lignite humic acid.
4. The method for preparing a building material having an electromagnetic wave absorption function according to claim 1, wherein: the roasted material is finely ground until the mass percentage content of the particle size which meets the particle size of less than 500 meshes is not less than 99 percent, and the specific surface area is not less than 4000cm2/g。
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