CN110526584B - Method for preparing porous microcrystalline material by using crystalline silicon cutting waste and coal gangue and application - Google Patents

Method for preparing porous microcrystalline material by using crystalline silicon cutting waste and coal gangue and application Download PDF

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CN110526584B
CN110526584B CN201910953697.7A CN201910953697A CN110526584B CN 110526584 B CN110526584 B CN 110526584B CN 201910953697 A CN201910953697 A CN 201910953697A CN 110526584 B CN110526584 B CN 110526584B
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coal gangue
microcrystalline material
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porous microcrystalline
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曹建尉
邹传明
王志
王东
赵明智
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Institute of Process Engineering of CAS
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    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/06Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/08Other methods of shaping glass by foaming
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    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
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    • 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
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    • 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
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0063Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
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    • C03C11/007Foam glass, e.g. obtained by incorporating a blowing agent and heating

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Abstract

The invention relates to a method for preparing a porous microcrystalline material by using crystalline silicon cutting waste and coal gangue and application thereof. The porous microcrystalline material is prepared from the following raw materials: 70.0-85.0 wt% of coal gangue, 10.0-15.0 wt% of feldspar, 2.0-10.0 wt% of crystalline silicon cutting waste, 2.0-8.0 wt% of soda ash and 0-5.0 wt% of foaming agent. The porous microcrystalline material prepared by the invention has the characteristics of light weight, wear resistance, acid and alkali corrosion resistance, good chemical stability, high strength, rapid cooling and heating resistance, good thermal insulation performance, sound insulation, easy cutting and the like, and has the advantages of low comprehensive cost, reusability and the like. The material can be widely applied to key materials in the fields of architectural decoration, battery pole plates, heat insulation, noise reduction, shock prevention and the like, and heat insulation of pipelines, storage tanks and heat exchange systems in the mechanical field.

Description

Method for preparing porous microcrystalline material by using crystalline silicon cutting waste and coal gangue and application
Technical Field
The invention belongs to the technical field of porous material preparation, and particularly relates to a method for preparing a porous microcrystalline material by using crystalline silicon cutting waste and coal gangue and application of the porous microcrystalline material.
Background
On the one hand, in the traditional energy field, China is a big coal country, the annual average coal production consumption amount reaches hundred million tons, and the environmental destruction caused by mining is increasingly paid attention by people. By 2017, according to incomplete statistics, the accumulated amount of the coal gangue in China reaches 45 hundred million tons, and the quantity of the coal gangue is increased by 1.5-2.0 hundred million tons every year. In the process of coal utilization, a large amount of coal gangue is generated, the surrounding living environment is damaged, the surrounding ecological pollution is caused, a large amount of land is occupied, geological disasters and water body pollution are easily caused, and the health and the life of the surrounding masses are seriously influenced. Therefore, the development of the green and high-added-value resource utilization of the coal gangue has very important significance.
On the other hand, in the field of new energy, China is rapidly developed in recent years, particularly, the development of the photovoltaic industry is quite rapid, and in 2017, the new photovoltaic loading capacity of China reaches 53.06GW, which is increased by 53.62% on a par with the new photovoltaic loading capacity. With the wide application of distributed photovoltaic in recent years, photovoltaic installation is coming to a new growth point. The domestic polycrystalline silicon yield in 2017 is 24.2 ten thousand tons, which exceeds the global yield by 50 percent. A large amount of crystalline silicon cutting waste materials are generated in the production process of the photovoltaic polycrystalline silicon material, and resource utilization is urgently needed.
Porous microcrystalline materials are considered to be one of the most advanced thermal insulation materials, having low average density, high material strength and excellent insulating ability, flame retardancy, high chemical resistance, low water absorption and almost unlimited service life (as opposed to organic and fibrous insulation materials), significantly expanding the field of application of porous materials. Porous microcrystalline materials can be used for: (1) load-bearing walls, ceilings, enclosure walls and internal partition walls of buildings; (2) cryogenic pipelines, equipment, vessels and storage tanks; (3) medium and high temperature pipes, equipment; (4) hot oil and hot asphalt storage tanks; (5) a fluid heat exchange system; (6) sound insulation and absorption walls such as compressors, fan houses and the like; (7) the composite thermal insulation system is operated under special conditions.
CN103708731B discloses a nickel slag porous microcrystal material and a preparation method thereof. Smelting ferronickel waste slag as main material and SiO2、CaCO3、Na2CO3、ZnO、K2CO3The additives and the clarifying agent are auxiliary materials, but the porous material is prepared by only using a single nickel-iron alloy slag.
In conclusion, the porous microcrystalline material is prepared by using the coal gangue and the crystalline silicon cutting waste as main raw materials, and the innovation is that the crystalline silicon cutting waste and the coal gangue are cooperatively used, wherein SiC in the crystalline silicon cutting waste can be used as a foaming agent, and the solid Si particles have the effect of promoting the uniform distribution of a batch thermal field; the coal gangue can be used as a raw material and a part of fuel, and the coal gangue can be used for producing low-cost high-added-value products and has obvious economic, environmental and social benefits.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to prepare a porous microcrystalline material by utilizing coal gangue and crystalline silicon cutting waste materials in a large quantity and high resource utilization manner, and simultaneously solves the problem of uneven thermal field of the porous microcrystalline material in the heating foaming process by utilizing the high heat conduction characteristic of Si particles, and provides a method for preparing the porous microcrystalline material by the cooperation of the coal gangue and the crystalline silicon cutting waste materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a porous microcrystalline material prepared by combining crystal silicon cutting waste with coal gangue, wherein the raw material of the porous microcrystalline material consists of the following components:
Figure BDA0002226576910000021
the sum of the total mass percent of the raw materials of the porous microcrystalline material is 100%.
The coal gangue content is, for example, 72 wt%, 74 wt%, 75 wt%, 76 wt%, 78 wt%, 80 wt%, 81 wt%, 82 wt%, 84 wt%, or the like; the content of the feldspar is, for example, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or the like; the content of the crystalline silicon cutting waste material is, for example, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, or the like; the content of the soda ash is, for example, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, or the like; the blowing agent is present in an amount of, for example, 0.2 wt%, 0.5 wt%, 0.8 wt%, 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, or 4.5 wt%, etc.
The method utilizes the coal gangue and the crystalline silicon cutting waste as main raw materials to prepare the microcrystalline material, and takes SiC in the crystalline silicon cutting waste as a foaming agent in the preparation process, so that the raw material cost of the foaming agent is obviously reduced; solid Si particles in the crystalline silicon cutting waste are raw materials, have the effect of adjusting the uniformity of a thermal field, can promote the basic batch of the porous microcrystalline material to be uniformly heated in the heating process, and improve the uniformity of pores in the obtained porous microcrystalline material; in the preparation process, the coal gangue is both a raw material and a fuel, so that the production cost of the porous microcrystalline material can be reduced, the pollution of industrial solid wastes to the environment can be reduced, and the preparation method has remarkable economic, environmental and social benefits.
Preferably, the composition of the crystalline silicon cutting waste material is as follows:
Figure BDA0002226576910000031
the sum of the total mass percentages of the components of the crystalline silicon cutting waste is 100%.
The content of the polyethylene glycol is, for example, 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or the like; the content of SiC is, for example, 22 wt%, 25 wt%, 28 wt%, 30 wt%, 32 wt%, 35 wt%, 36 wt%, 38 wt%, or the like; the Si content is, for example, 42 wt%, 45 wt%, 48 wt%, 50 wt%, 52 wt%, 55 wt%, 56 wt%, 58 wt%, 60 wt%, 62 wt%, 65 wt%, 66 wt%, 68 wt%, or the like; the SiO2Such as 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or the like; said Fe2O3E.g., 1 wt%, 2 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or the like; the other trace is impurities with extremely low content.
Preferably, the coal gangue consists of:
Figure BDA0002226576910000041
the sum of the total mass percentages of the coal gangue is 100%.
SiO in the coal gangue2E.g., 50.2 wt%, 50.5 wt%, 50.8 wt%, 51 wt%, 51.2 wt%, 51.5 wt%, 52 wt%, 52.5 wt%, 53 wt%, 53.5 wt%, 54 wt%, or 54.5 wt%, etc(ii) a Al in the coal gangue2O3E.g., 20.2 wt%, 20.5 wt%, 20.8 wt%, 21 wt%, 21.2 wt%, 21.5 wt%, 22 wt%, 22.5 wt%, 23 wt%, 23.5 wt%, 24 wt%, or 24.5 wt%, etc.; fe in the coal gangue2O3E.g., 4.5 wt%, 5 wt%, 5.5 wt%, 6 wt%, 6.5 wt%, 7 wt%, 7.5 wt%, 8 wt%, 8.5 wt%, or the like; the content of CaO in the coal gangue is, for example, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, 5 wt%, 5.5 wt%, or the like; SO in the coal gangue3E.g., 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, 5 wt%, 5.5 wt%, 6 wt%, 6.5 wt%, 7 wt%, 7.5 wt%, 7.8 wt%, or the like; k in the coal gangue2An O content such as 1.2 wt%, 1.5 wt%, 1.6 wt%, 1.8 wt%, 2 wt%, 2.2 wt%, 2.5 wt%, 2.6 wt%, or 2.8 wt%, etc.; TiO in the coal gangue2E.g., 1.1 wt%, 1.2 wt%, 1.3 wt%, 1.4 wt%, 1.5 wt%, 1.6 wt%, 1.7 wt%, 1.8 wt%, or 1.9 wt%, etc.; the content of MgO in the coal gangue is, for example, 0.3 wt%, 0.5 wt%, 0.6 wt%, 0.8 wt%, 1 wt%, 1.2 wt%, 1.5 wt%, 1.6 wt%, 1.8 wt%, or the like; na in the coal gangue2O content such as 0.1 wt%, 0.2 wt%, 0.3 wt%, or 0.4 wt%, etc.; p in the coal gangue2O5E.g., 0.12 wt%, 0.14 wt%, 0.15 wt%, 0.2 wt%, 0.22 wt%, 0.24 wt%, 0.25 wt%, or 0.28 wt%, etc.; the other trace is impurities with extremely low content.
Preferably, the coal gangue has a loss on ignition of 5.0 to 40.0 wt%, such as 6 wt%, 8 wt%, 10 wt%, 12 wt%, 15 wt%, 18 wt%, 20 wt%, 22 wt%, 25 wt%, 30 wt%, 35 wt%, or the like.
Preferably, the foaming agent comprises any one of carbon black, limestone powder, dolomite powder, phlogopite, graphite and manganese dioxide or a combination of at least two of the same.
Preferably, the mass ratio of the carbon black, the limestone powder, the dolomite powder, the phlogopite, the graphite and the manganese dioxide is (0-1.0): 1.0-2.0, such as 0.2:0.1:0.5:0.3:0.4:1.8, 0.1:0.1:0.3:0.7:0.2:1.5, 0.3:0.2:0.1:0.8: 0.1.6, 0.4:0.2:0.1:0.9:0.1:1.7, 0.1:0.2:0.8:0.1:0.6:1.9, 0.5:0.6:0.3:0.8:0.1: 0.1.9, 0.1:0.8: 0.1:0.9: 0.8:0.1: 0.9: 0.0.9: 0.8:0.1: 0.0.0.9: 0.0.9: 0.0.0.9: 0.0.9: 0.0.0.0..
Preferably, the feldspar comprises any one of albite, potassium feldspar, anorthite, celsian and microcline feldspar or the combination of at least two of the albite, the potassium feldspar, the anorthite, the celsian and the microcline feldspar.
Preferably, the mass ratio of albite, potash feldspar, anorthite, celsian and celsian is (0-1.0): (1.0-2.0), for example, 0.2:0:0:0:0:0, 0.1:0:0:0:0, 0.3:0.2:0.1:0.8:0.2:1.6, 0.4:0.2:0.1:0.9:0.1:1.7, 0.1:0.2:0.8:0.1:0.6:1.9, 0.5:0.6:0.3:0.8:0.1:1.4 or 0:0.1: 0.2.
The second purpose of the invention is to provide a method for preparing a porous microcrystalline material by using the crystalline silicon cutting waste and the coal gangue, which comprises the following steps:
(1) crushing the coal gangue waste, and sieving with a 30-mesh sieve;
(2) uniformly mixing 70.0-85.0 wt% of coal gangue, 10.0-15.0 wt% of feldspar, 2.0-8.0 wt% of soda ash, 2.0-10.0 wt% of crystalline silicon cutting waste and 0-5.0 wt% of foaming agent in percentage by mass, and adding a proper amount of water;
(3) adding the coal gangue, the crystal silicon cutting waste, the feldspar, the soda ash and the foaming agent into a ball mill according to the proportion of the raw materials, and carrying out wet ball milling to obtain uniform slurry;
(4) drying the ball-milled uniform slurry to obtain powder, filling the powder into a mold, and feeding the mold with the powder into a heat treatment kiln for preheating, firing and demolding to obtain a blank plate;
(5) and (4) performing thickness setting and cutting on the fired blank plate, and finally packaging and warehousing the finished product.
Preferably, the drying temperature in step (4) is 100 to 300 ℃, such as 120 ℃, 150 ℃, 160 ℃, 180 ℃, 200 ℃, 220 ℃, 250 ℃, 260 ℃ or 280 ℃.
Fig. 1 is a flow chart of a preparation process of the microcrystalline glass provided by the present invention, and it can be seen from the flow chart that porous microcrystalline glass (i.e. porous microcrystalline material) can be obtained by mixing raw materials, and performing ball milling, charging (molding), and firing (sintering and foaming) processes.
Preferably, the firing described in step (4) is performed according to the following sintering procedure:
a preheating stage: raising the temperature in the furnace from room temperature to 350-450 ℃, wherein the raising rate is 5-20 ℃/min, such as 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃, 420 ℃, 430 ℃ or 440 ℃ and the like; for example, 6 deg.C/min, 8 deg.C/min, 10 deg.C/min, 12 deg.C/min, 14 deg.C/min, 15 deg.C/min, 16 deg.C/min, 18 deg.C/min, or 19 deg.C/min.
And (3) sintering stage: raising the temperature in the furnace from 350-450 ℃ to 920-980 ℃ at a rate of 5-15 ℃/min, such as 930 ℃, 940 ℃, 950 ℃, 960 ℃ or 970 ℃ and the like; for example, 6 deg.C/min, 7 deg.C/min, 8 deg.C/min, 9 deg.C/min, 10 deg.C/min, 11 deg.C/min, 12 deg.C/min, 13 deg.C/min, or 14 deg.C/min.
And (3) foaming stage: the temperature in the furnace is increased from 920-980 ℃ to the highest firing temperature, and the heating rate is 5-10 ℃/min, such as 6 ℃/min, 7 ℃/min, 8 ℃/min or 9 ℃/min.
And (3) annealing stage: and (4) reducing the temperature in the furnace from the highest firing temperature to room temperature, and cooling along with the furnace.
Preferably, the highest firing temperature in the foaming stage is 1100-1300 ℃, and the heat is preserved for 0.3-2.0 h at the highest firing temperature, such as 1120 ℃, 1150 ℃, 1180 ℃, 1200 ℃, 1220 ℃, 1250 ℃ or 1280 ℃ and the like; for example, 0.5h, 0.6h, 0.8h, 1h, 1.2h, 1.4h, 1.5h, 1.6h, 1.8h, etc.
In the present invention, the various heat treatment stages of the sintering procedure have the following meanings:
a preheating stage: the stage is an evaporation stage, mainly mechanical water and adsorbed water are removed, and the powder does not undergo chemical change, but only undergoes physical changes such as volume shrinkage, porosity increase and the like.
And (3) sintering stage: the stage is an oxidative decomposition stage, and the main chemical changes of the powder are the removal of structural water, the decomposition and oxidation of compounds such as organic matters, carbonate, SiC and the like contained in a blank body and the crystal form transformation.
And (3) foaming stage: the main change in this stage is that the powder in the green body is melted to form a liquid phase, and the green body is gradually compacted. On the one hand, the crystal is recrystallized in the liquid phase to form a new crystal and continuously grows in the liquid phase; at the same time, the gas generated by the foaming agent forms bubbles in the liquid phase to form a gas-liquid two-phase composite.
And (3) annealing stage: and (3) reducing the temperature in the kiln from the highest firing temperature to room temperature, and cooling along with the kiln to obtain the porous microcrystalline material. At this stage, the viscosity of the glass-crystal composite solid phase in the product is increased, the plastic state is converted into the solid state, and the hardness and the strength are increased to the maximum.
The shape of the porous microcrystalline material is a plate shape or a cylindrical shape or a curved shape, or any other shape processed according to actual needs.
The invention also aims to provide the application of the porous microcrystalline material prepared by combining the crystalline silicon cutting waste and the coal gangue, which is used in any one or the combination of at least two of the fields of buildings, pipeline equipment, sound insulation, sound absorption walls and composite heat insulation systems.
Compared with the prior art, the invention has the following beneficial effects:
(1) the high-value utilization of the new energy solid waste and the traditional energy solid waste in cooperation with resource utilization is realized:
the coal gangue is used as a main raw material to produce the porous microcrystalline material with high added value, the mixing amount of the coal gangue in the porous microcrystalline material can be adjusted within the range of 70-85 wt%, and the coal gangue is both a raw material and a fuel, so that the production cost of the porous microcrystalline material can be reduced, and the pollution of industrial solid wastes to the environment can be reduced.
(2) The design utilizes the multiple functions of the main components of the crystal silicon cutting waste material:
si particles in the crystal silicon cutting waste are raw materials, and have the effect of adjusting the uniformity of a thermal field, so that the basic batch of the porous microcrystalline glass material is promoted to be uniformly heated in the heating process, and the uniformity of pores is improved; SiC in the crystalline silicon cutting waste can be used as a foaming agent, so that the raw material cost of the foaming agent is obviously reduced.
(3) Develops a sintering process of the porous microcrystalline material by a one-step method:
the invention completes the processes of melting, foaming, crystallizing, annealing and the like of the porous microcrystalline material through one-time sintering, abandons the sintering process of a two-step method that the traditional porous microcrystalline material is firstly prepared into foam glass and then crystallized, and obviously shortens the sintering period.
Drawings
Fig. 1 is a flow chart of a preparation process of the porous glass ceramics provided by the invention.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The composition of the coal gangue used in this example is: SiO 22Is 53 wt% of Al2O3Is 25 wt% of Fe2O3Is 5 wt%, CaO is 5 wt%, SO3Is 6 wt%, K22% by weight of O, TiO22 wt%, MgO 1.7 wt%, Na2O content 0.2 wt%, P2O5The content of (A) is 0.1 wt%, and the content of impurities is trace; the content of polyethylene glycol in the crystalline silicon cutting waste material is 10 wt%, the content of SiC is 30 wt%, the content of Si is 50 wt%, and SiO is2Is 5 wt% of Fe2O3Is 5 wt% and the impurity content is a trace amount.
(1) Uniformly mixing 79 wt% of coal gangue, 11 wt% of feldspar, 4 wt% of soda ash, 3 wt% of crystal silicon cutting waste and 3 wt% of foaming agent, adding the mixture into a ball mill, and carrying out wet ball milling for 3 hours to obtain slurry with the ball-milled fineness of 200 meshes, wherein the foaming agent is limestone powder and manganese dioxide (the mass ratio is 1: 1);
(2) drying the ball-milled slurry, and controlling the temperature to be 120 ℃ to obtain powder;
(3) and (3) feeding the mold with the powder distributed into a furnace for heat treatment, and performing the following procedures:
a preheating stage: heating the temperature in the heat treatment furnace from room temperature to 400 ℃, wherein the heating rate is 20 ℃/min, and the heat preservation time is 30 min;
and (3) sintering stage: heating the temperature in the heat treatment furnace from 400 ℃ to 960 ℃, wherein the heating rate is 15 ℃/min, and the heat preservation time is 30 min;
and (3) foaming stage: heating the temperature in the heat treatment furnace from 960 ℃ to 1160 ℃ of the maximum firing temperature, wherein the heating rate is 10 ℃/min, and the heat preservation time is 30 min;
and (3) annealing stage: reducing the temperature in the heat treatment furnace from the highest firing temperature to room temperature;
(4) and polishing and cutting the fired blank plate, and finally packaging and warehousing the finished product.
Example 2
The composition of the coal gangue used in this example is: SiO 22Is 55 wt% of Al2O3Is 20 wt% of Fe2O38 wt% of (B), 6 wt% of CaO, and SO3Is 5 wt%, K22% by weight of O, TiO22.4 wt%, MgO 1 wt%, Na2O content 0.5 wt%, P2O5The content of (A) is 0.1 wt%, and the content of impurities is trace; the content of polyethylene glycol in the crystalline silicon cutting waste material is 5 wt%, the content of SiC is 25 wt%, the content of Si is 50 wt%, and SiO is2Is 10 wt% of Fe2O3Is 10 wt% and the impurity content is a trace amount.
(1) Uniformly mixing 76 wt% of coal gangue, 14.5 wt% of feldspar, 4.5 wt% of soda ash, 2.5 wt% of crystal silicon cutting waste and 2.5 wt% of foaming agent, adding the mixture into a ball mill, and carrying out wet ball milling for 3 hours to obtain slurry with the ball-milled fineness of 200 meshes, wherein the foaming agent is dolomite powder and manganese dioxide (the mass ratio is 1: 2);
(2) drying the ball-milled slurry at the temperature of 150 ℃ to obtain powder;
(3) and (3) feeding the mold with the powder distributed into a furnace for heat treatment, and performing the following procedures:
a preheating stage: heating the temperature in the heat treatment furnace from room temperature to 350 ℃, wherein the heating rate is 10 ℃/min, and the heat preservation time is 1 h;
and (3) sintering stage: heating the temperature in the heat treatment furnace from 350 ℃ to 920 ℃, wherein the heating rate is 10 ℃/min, and the heat preservation time is 1.5 h;
and (3) foaming stage: heating the temperature in the heat treatment furnace from 920 ℃ to 1120 ℃ of the maximum firing temperature, wherein the heating rate is 8 ℃/min, and the heat preservation time is 1.2 h;
and (3) annealing stage: reducing the temperature in the heat treatment furnace from the highest firing temperature to room temperature, and cooling along with the furnace;
(4) and polishing and cutting the fired blank plate, and finally packaging and warehousing the finished product.
Example 3
The composition of the coal gangue and the crystal silicon cutting waste used in this example was the same as in example 1.
(1) Uniformly mixing 81 wt% of coal gangue, 9.5 wt% of feldspar, 4.5 wt% of soda ash, 2.5 wt% of crystal silicon cutting waste and 2.5 wt% of foaming agent, wherein the foaming agent is phlogopite and manganese dioxide (the mass ratio is 0.5:2), and obtaining a mixed material;
(2) drying the ball-milled slurry, and controlling the temperature to be 200 ℃ to obtain powder;
(3) and (3) feeding the mold with the powder distributed into a furnace for heat treatment, and performing the following procedures:
a preheating stage: heating the temperature in the heat treatment furnace from room temperature to 450 ℃, wherein the heating rate is 5 ℃/min, and the heat preservation time is 0.3 h;
and (3) sintering stage: the temperature in the heat treatment furnace is increased from 450 ℃ to 980 ℃, the temperature increase rate is 5 ℃/min, and the heat preservation time is 0.3 h;
and (3) foaming stage: the temperature in the heat treatment furnace is increased from 980 ℃ to 1250 ℃ which is the highest firing temperature, the heating rate is 5 ℃/min, and the heat preservation time is 0.5 h;
and (3) annealing stage: reducing the temperature in the heat treatment furnace from the highest firing temperature to room temperature, and cooling along with the furnace;
(4) and polishing and cutting the fired blank plate, and finally packaging and warehousing the finished product.
Example 4
The difference from the example 1 is that the coal gangue content in the step (1) is 72 wt%, the feldspar content is 15 wt%, the soda ash content is 8 wt%, the crystal silicon cutting waste material content is 3 wt%, and the foaming agent content is 2 wt%.
Example 5
The difference from the example 1 is that the coal gangue content in the step (1) is 80 wt%, the feldspar content is 10 wt%, the soda ash content is 4 wt%, the crystal silicon cutting waste material content is 3 wt%, and the foaming agent content is 3 wt%.
The density of the porous microcrystalline glass obtained in the embodiment of the invention is less than 720kg/m3Compressive strength of more than 7.0MPa, heat conductivity coefficient of less than or equal to 0.06W/m.k, and acid resistance k<0.12% alkali resistance<0.05 percent, light weight, acid and alkali corrosion resistance, high strength, rapid cooling and heating resistance, fire resistance, good heat preservation performance, easy cutting and the like. The composite material can be widely used for heat insulation, noise reduction, shock prevention and the like in the architectural decoration field and heat insulation and preservation of pipelines, storage tanks and heat exchange systems in the industrial field.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (12)

1. A porous microcrystalline material prepared by combining crystal silicon cutting waste with coal gangue is characterized in that the raw material of the porous microcrystalline material consists of the following components:
Figure FDA0002635305220000011
the sum of the total mass percent of the raw materials of the porous microcrystalline material is 100%.
2. The porous microcrystalline material as claimed in claim 1, wherein the composition of the crystalline silicon cutting waste is:
Figure FDA0002635305220000012
other trace amounts;
the sum of the total mass percentages of the components of the crystalline silicon cutting waste is 100%.
3. The porous microcrystalline material according to claim 1 or 2, wherein the coal gangue has a composition of:
Figure FDA0002635305220000013
Figure FDA0002635305220000021
other trace amounts;
the sum of the total mass percentages of the coal gangue is 100%.
4. The porous microcrystalline material according to claim 1, wherein the loss on ignition of the coal gangue is 5.0-40.0 wt%.
5. The porous microcrystalline material of claim 1 wherein the blowing agent comprises any one of carbon black, limestone powder, dolomite powder, phlogopite, graphite and manganese dioxide or a combination of at least two thereof.
6. The porous microcrystalline material according to claim 5, wherein the mass ratio of the carbon black, limestone powder, dolomite powder, phlogopite, graphite and manganese dioxide is (0-1.0): 0-1.0: (0-1.0): 1.0-2.0).
7. The porous microcrystalline material of claim 1 wherein the feldspar comprises one of albite, potassium feldspar, anorthite, celsian, microcline feldspar, or a combination of at least two of these.
8. The method for preparing the porous microcrystalline material by using the crystalline silicon cutting waste and the coal gangue as the raw materials according to claim 1, wherein the preparation method comprises the following steps:
(1) crushing the coal gangue waste, and sieving with a 30-mesh sieve;
(2) uniformly mixing 70.0-85.0 wt% of coal gangue, 10.0-15.0 wt% of feldspar, 2.0-8.0 wt% of soda ash, 2.0-10.0 wt% of crystalline silicon cutting waste and 0-5.0 wt% of foaming agent in percentage by mass, and adding a proper amount of water;
(3) adding the coal gangue, the crystal silicon cutting waste, the feldspar, the soda ash and the foaming agent into a ball mill according to the proportion of the raw materials, and carrying out wet ball milling to obtain uniform slurry;
(4) drying the ball-milled uniform slurry to obtain powder, filling the powder into a mold, and feeding the mold with the powder into a heat treatment kiln for preheating, firing and demolding to obtain a blank plate;
(5) and (4) performing thickness setting and cutting on the fired blank plate, and finally packaging and warehousing the finished product.
9. The method according to claim 8, wherein the drying temperature in the step (4) is 100 to 300 ℃.
10. The method according to claim 8, wherein the firing in the step (4) is performed according to the following sintering procedure:
a preheating stage: heating the temperature in the furnace from room temperature to 350-450 ℃, wherein the heating rate is 5-20 ℃/min;
and (3) sintering stage: raising the temperature in the furnace from 350-450 ℃ to 920-980 ℃ at a rate of 5-15 ℃/min;
and (3) foaming stage: raising the temperature in the furnace from 920-980 ℃ to the maximum firing temperature, wherein the temperature raising rate is 5-10 ℃/min;
and (3) annealing stage: and (4) reducing the temperature in the furnace from the highest firing temperature to room temperature, and cooling along with the furnace.
11. The method according to claim 10, wherein the foaming stage is carried out at a maximum firing temperature of 1100 to 1300 ℃ and the temperature is maintained at the maximum firing temperature for 0.3 to 2.0 hours.
12. Use of the crystalline silicon cutting waste in combination with coal gangue as defined in any one of claims 1 to 7 for preparing a porous microcrystalline material for any one or a combination of at least two of the fields of construction, piping equipment, sound insulation, sound-absorbing walls and composite thermal insulation systems.
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