CN117466621A - Hollow ultra-light ceramsite based on oil-based rock debris and preparation method thereof - Google Patents
Hollow ultra-light ceramsite based on oil-based rock debris and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
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- 238000000034 method Methods 0.000 claims abstract description 31
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- 239000011737 fluorine Substances 0.000 claims description 23
- 229910052731 fluorine Inorganic materials 0.000 claims description 23
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 22
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 22
- 241001330002 Bambuseae Species 0.000 claims description 22
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 22
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- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 claims description 11
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- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 3
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- 229910008284 Si—F Inorganic materials 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052661 anorthite Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- 239000011019 hematite Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
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Classifications
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1324—Recycled material, e.g. tile dust, stone waste, spent refractory material
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- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
- C04B33/1322—Red mud
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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
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- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1328—Waste materials; Refuse; Residues without additional clay
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- C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- 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
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- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The invention discloses a hollow ultra-light ceramsite based on oil-based rock debris and a preparation method thereof, and relates to the field of ceramsites; mixing the foaming agent microspheres with the mixed raw material by adding water to prepare green pellets; roasting the green pellets by adopting a step-by-step roasting method, and cooling to obtain the hollow ultra-light ceramsite. The raw materials adopted by the invention are industrial wastes, the raw material cost is low, the aim of cooperatively disposing the oil-based rock debris residues by multiple solid wastes is fulfilled, the difficult problems of high disposal cost, large accumulation amount, difficult disposal, low utilization rate, difficult popularization and application of resource products and the like of the oil-based rock debris residues are solved, and the method has very important significance in expanding the resource utilization path of the oil-based rock debris residues and guaranteeing the green development of shale gas.
Description
Technical Field
The invention relates to the field of ceramsite, in particular to hollow ultra-light ceramsite based on oil-based rock debris and a preparation method thereof.
Background
The ceramsite is used as an artificial lightweight aggregate, and can provide certain strength under the premise of ensuring the lightweight property of the ceramsite due to the characteristics of dense internal pores and hard and compact outer layers, can replace natural aggregates such as concrete broken stones and pebbles, and has the functions of heat insulation, shock resistance, fire resistance, sound insulation, noise reduction and the like, however, most of traditional ceramsite is of a porous structure, and the problems of leakage and the like are often caused by higher water absorption rate in the use process. Therefore, in order to avoid the defects caused by the porous structure, the hollow ceramsite with the central macroporous structure is researched and developed, and compared with the traditional porous ceramsite, the hollow ceramsite with the central macroporous structure has the characteristics of lower water absorption, better heat preservation and sound insulation effects, smaller dead weight and the like, and has a wide application prospect. Currently, natural raw materials for producing ceramsite have been gradually replaced by industrial waste materials, such as: tailings, municipal sludge, fly ash, and the like. The related researches find that oil-based rock debris residues are similar to the industrial solid waste components and all contain a large amount of SiO 2 And Al 2 O 3 The components have the potential of firing ceramsite.
The application number is 201911283048.7, a preparation method of hollow ceramsite by using clay and fly ash is disclosed, the method uses the heated decomposable, combustible or soluble substances as spherical core made of material, the spherical core outer layer is wrapped by polypropylene or carbon, and the hollow shell is formed after high-temperature sintering, so that the bulk density is 350-500kg/m 3 And hollow ceramsite with water absorption rate of 12-15%.
The application number is 201210462747.X, the lightweight hollow ceramsite consists of ceramic forming materials and template materials, wherein the ceramic forming materials consist of waste paper papermaking dry sludge, fly ash and clay, and the template materials are polyphenyl foam particles; the shape of the obtained lightweight hollow ceramsite is spherical or spheroid, the middle cavity is also spherical or spheroid, and the middle cavity is separated from the outside by a layer of ceramic structure with the wall thickness of 0.5-2.5 mm; the light hollow ceramsite has a cylinder pressure of 3-5MPa and a bulk density of 300-500kg/m 3 。
The prior art has added a sacrificial template material to prepare the hollow ceramsite, and the method uses a large amount of template material, thereby not only increasing the production cost, but also effectively combining the template material with the ceramic forming material, and generating waste polluting the environment in the template preparation process. Meanwhile, the existing ceramic material composition still contains natural minerals such as clay, which is unfavorable for sustainable development strategy.
Disclosure of Invention
The invention aims to provide a preparation method of hollow ultra-light ceramsite based on oil-based rock debris, which is characterized in that oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag, red mud and foaming agent microspheres are prepared into hollow ceramsite with small density, high strength, low water absorption and closed cavities inside on the basis of not adding a sacrificial template material.
In order to achieve the above object, the present invention comprises the steps of: the method is characterized by comprising the following steps of:
s1, grinding and mixing oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag and red mud to obtain mixed raw materials;
s2, mixing the foaming agent microspheres with the mixed raw material by adding water to prepare green pellets;
s3, roasting the green pellets by adopting a step-by-step roasting method, and cooling the green pellets along with a furnace to obtain hollow ultra-light ceramsite; the firing system of the step firing method comprises three stages, wherein the first stage is to heat up to 400-600 ℃ at the room temperature, and keep the temperature for 10-30min, and the heating rate is 8-15 ℃/min; the second stage is to raise the temperature to 800-1000 ℃ at 400-600 ℃ and the heating rate is 8-15 ℃/min; the third stage is to heat the temperature of 800-1000 ℃ to 1050-1150 ℃ and keep the temperature at 1050-1150 ℃ for 5-20min, and the heating rate is 5-10 ℃/min. Preferably, the first stage is to heat up to 500 ℃ at room temperature and keep the temperature for 20min, and the heating rate is 10 ℃/min; the second stage is to raise the temperature to 950 ℃ at 500 ℃ and the heating rate is 10 ℃/min; the third stage is to heat up to 1050-1150 deg.C at 950 deg.C and keep the temperature at 1050-1150 deg.C for 10min at a heating rate of 5 deg.C/min.
In the step S1, oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag and red mud are dried, mixed and ground for 0.8-1.5h through a stirring ball mill, the rotation speed of a cylinder is 150-350r/min, the rotation speed of a stirring shaft is 900-1200r/min, and mixed raw materials are obtained through a screen of 0.075mm after grinding.
Specifically, in the step S1, the characteristics of the high-carbon chromium iron slag, the fluorine-containing sludge and the red mud are utilized to play a role of a sintering aid in the ceramic matrix, the ceramic performance can be optimized without adding the sintering aid, the liquid phase generation temperature is promoted to be reduced, the generated gas can be wrapped by the liquid phase at a lower sintering temperature, and a pore foundation is provided for realizing the ceramic cavity structure.
Meanwhile, the high-carbon chromium iron slag also contains MgO component which can be mixed with the rock debris residue and Al rich in red mud 2 O 3 、SiO 2 The components are adapted, the formation of forsterite crystals is promoted, and the characteristics of good thermal stability, stable crystal structure, high corrosion resistance and the like of the crystalline phase are utilized to further improve the performance of the hollow ceramsite.
In addition, the red mud contains a certain clay component, so that the addition of a binder can be avoided; secondly, the fluorine-containing sludge contains CaF 2 It is added into the ceramsite matrix as a crystal nucleus agent, because of F - Radius (0.13)6 nm) and O 2- Is very close to the radius (0.140 nm) and therefore F - Can easily replace O in glass network 2- According to the electricity price balance rule, two F - Can replace one O 2- converting-Si-O-into-Si-F and existing as non-bridging oxygen in the network, while breakage of the silica network reduces the viscosity of the glass, destroying the network structure of glassy anions, thus F during crystallization - Can be separated out from the melt first, provide nucleation sites for the separation of crystals, reduce the generation temperature of the crystals, and finally promote the aluminosilicate crystals such as celsian, forsterite and the like in the ceramic matrix, thereby realizing the further improvement of the physical properties of the hollow ultra-light ceramic.
Further, the step-by-step roasting comprises three stages, wherein in the first stage, the temperature of the ceramsite is gradually increased to 400-600 ℃ from room temperature, the heating rate is set to 8-15 ℃/min, and the temperature is kept for 10-30min, and the purpose of the stage is to promote the evaporation of residual crystal water in the raw materials, the decomposition of organic matters and the like, so as to avoid the cracking of a blank, and the ceramsite contains pores left by the reaction and decomposition of part of components;
in the second stage, the temperature of the ceramsite is increased from 400-600 ℃ to 800-1000 ℃, the temperature increasing rate is set to 8-15 ℃/min, heat is not preserved, liquid phase and gas phase in a ceramsite matrix are gradually generated in the temperature increasing process, the foaming agent microspheres start to participate in the reaction and generate a small amount of gas, at the moment, small pores communicated with the inside and the outside are formed in the ceramsite, and a pore foundation is laid for the formation of a cavity structure in the third stage;
in the third stage, the temperature of the ceramsite is increased from 800-1000 ℃ to the target temperature, the temperature increasing rate in the stage is set to 5-10 ℃/min, the temperature is kept for 5-20min, the foaming agent microspheres undergo a severe reaction, a large number of macropores wrapped by liquid phase are formed in the ceramsite matrix, at the moment, the liquid phase viscosity in the ceramsite is higher than the liquid phase viscosity in the ceramsite due to the fact that the temperature of the periphery of the ceramsite is higher than the internal temperature, gas generated in the ceramsite is not easy to disperse, the internal gas is easy to aggregate mutually to form a hollow structure of a ceramsite core, the pore structure generated in the periphery of the ceramsite pushes the liquid phase to expand outwards, the enamel of the periphery of the ceramsite gradually begins to promote the generated gas to be not easy to overflow, and finally the hollow ceramsite with a cavity structure and a porous ceramic structure periphery is formed.
Furthermore, the invention provides a preparation method of the foaming agent microsphere, which specifically comprises the following preparation steps:
drying the washed salt gypsum, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag, and grinding and mixing to obtain powder; wherein, the weight part ratio of the gypsum salt to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag is 3-5:1-2:3-5; the particle size of the ground powder is less than or equal to 5 mu m, so that the surface area of solid particles is increased, particle agglomeration is broken, the reaction rate of the foaming agent at high temperature is improved, and the reaction time is shortened.
Pouring the powder into a powerful mixer, adding atomized water, setting the rotating speed of a rotor of the powerful mixer to be 1200-2000r/min, setting the rotating speed of a cylinder to be 30-50r/min, and stopping working after the powerful mixer rotates for 5-15min to obtain microspheres;
the microspheres are placed in a vibrating screen and sequentially screened by screens with the mesh numbers of 18 meshes, 25 meshes, 40 meshes and 60 meshes to obtain three foaming agent microspheres, wherein the particle sizes of the three foaming agent microspheres are respectively X1, X2 and X3, and X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm.
In the step S2, the weight part ratio of the three foaming agent microspheres of X1, X2 and X3 is 0.5-4:2-4:2-6.
After the three foaming agent microspheres are mixed with the mixed raw materials by adding water, a granulating plate with the diameter of 12mm is adopted to obtain a green ball with the diameter of 11-13mm through blocking, extrusion and rolling.
The foaming agent microsphere is compounded by utilizing a plurality of solid waste-based foaming agents, and simultaneously, the foaming agent microsphere with different particle diameters is utilized to form particle grading so as to meet the requirement that the foaming agent forms different decomposition rates and foaming amounts under the conditions of different temperature ranges, and finally, a special pore structure is realized; the solid waste-based foaming agent mainly comprises a foaming component and a modifying component, and has the characteristics of Wen Ouan foaming, large gas production and the like, wherein the gypsum salt and the ceramic polishing slag are used as the foaming component to realize the gas production reaction under different temperature sections, the waste bamboo charcoal-based adsorbent is used as the modifying component to be matched with the foaming component in a matrix to accelerate the gas production reaction, foaming points can be provided for the ceramic granules in the second stage of ceramic granule roasting, a large number of pores which are communicated with each other and have different pore sizes are promoted, a pore foundation is laid for the formation of a cavity structure in the third stage, and hollow ceramic granules with the cavity structure and the periphery of the porous ceramic structure are formed through the action of the foaming agent microspheres in the firing process in the third stage.
The waste bamboo charcoal-based adsorbent is waste obtained by using bamboo charcoal as an adsorbent material, wherein the bamboo charcoal is a solid product obtained by thermally decomposing (carbonizing) bamboo under the conditions of high temperature and oxygen deficiency;
the salt gypsum is a byproduct generated in salt making industry or salt farm seawater concentration;
the ceramic polishing slag is polishing slag containing abrasive silicon carbide generated in the ceramic tile cutting and polishing process.
Furthermore, the invention also provides a second invention object, namely the hollow ultra-light ceramsite prepared by the preparation method, wherein the hollow ultra-light ceramsite comprises the following components in parts by weight: 40-60 parts of oil-based rock debris residues, 15-30 parts of high-carbon ferrochrome residues, 10-20 parts of fluorine-containing sludge, 10-20 parts of red mud and 6-10 parts of foaming agent microspheres.
The hollow ultra-light ceramsite prepared by the preparation method disclosed by the invention consists of a hollow inner core and a porous ceramic periphery, wherein the inner core of the hollow ultra-light ceramsite is in a hollow closed cavity structure and is in a sphere-like shape; the periphery is traditional porous ceramic structure, and it comprises a large amount of closed holes, and open hole quantity is few, has low water absorption characteristics simultaneously, and this hollow haydite structure is porous ceramic structure than traditional hollow haydite its periphery, has reduced the stress concentration phenomenon and open hole quantity when pressing and is few, and the water absorption is lower.
The hollow ultra-light ceramsite cylinder has a pressure of 4-6MPa and a bulk density of 400-500kg/m 3 The water absorption rate is 0.5-2%, the porosity is 55-65%, and meanwhile, the leaching values of heavy metal ions meet the limit requirements of GB 5985.3-2007 hazardous waste identification Standard leaching toxicity identification.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the hollow ultra-light ceramsite based on the oil-based rock debris and the preparation method thereof, the ultra-light ceramsite with the closed cavity structure is prepared by using a new route on the basis of not adding a sacrificial template material, and the defects that the existing template method is complex in preparation process, high in cost, heavy in pollution and difficult to realize industrial scale application are overcome;
the raw materials adopted by the invention are industrial wastes, the raw material cost is low, the aim of cooperatively disposing oil-based rock debris residues by multiple solid wastes is fulfilled, the difficult problems of high disposal cost, large accumulation amount, difficult disposal, low utilization rate, difficult popularization and application of resource products and the like of the oil-based rock debris residues are solved, and the method has very important significance in expanding the resource utilization path of the oil-based rock debris residues and guaranteeing the green development of shale gas;
the invention utilizes the fluorine-containing sludge to be rich in fluxing component and CaF 2 The ceramic particle is characterized in that the ceramic particle is added into a ceramic particle matrix to serve as a fluxing agent and a crystal nucleus agent, no sintering aid is required to be additionally added in the preparation process of the hollow ceramic particle, and the production cost is reduced while the sintering temperature of the ceramic particle is reduced and the crystal structure is optimized;
the foaming agent microsphere used in the invention is prepared by mixing the gypsum salt, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag, and has the characteristics of wide foaming temperature range, good gas production effect and the like, and has the advantages of abundant raw material sources, low cost, simple preparation process and good gas production performance;
the hollow ceramsite prepared by the invention consists of a hollow inner core and a porous outer periphery, wherein the inner core of the hollow ceramsite is in a hollow closed cavity structure and is in a sphere-like shape; the periphery is a traditional porous ceramic structure, compared with the traditional hollow ceramic particle, the stress concentration phenomenon of a single pore structure when being pressed can be reduced, the number of the open pores is small, the water absorption is lower, and meanwhile, the leaching values of heavy metal ions of the porous ceramic particle all meet the limiting requirements of GB 5985.3-2007 hazardous waste identification standard leaching toxicity identification.
Drawings
The accompanying drawings, which are included to provide a further understanding of embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiments of the invention. In the drawings:
FIG. 1 is an XRD pattern of hollow ultra-light ceramsite prepared in example 1 and examples 7-10;
FIG. 2 is a graph of the crystal microstructure of the hollow ultra-light ceramsite subjected to acid corrosion and an EDS energy spectrum of example 1, wherein (a) is the crystal microstructure of the ceramsite subjected to acid corrosion; (b) EDS spectra of celsian crystals; (c) EDS spectra of heavy-rock crystals;
FIG. 3 is a CT scan of hollow ultra-light ceramsite of example 1;
FIG. 4 is a CT scan of hollow ultra-light ceramsite of example 2.
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, but the present invention is not limited to the scope of the examples. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Example 1
In a dry state, weighing the materials according to the following parts by weight: 50 parts of oil-based rock debris residues, 25 parts of high-carbon ferrochrome slag, 15 parts of fluorine-containing sludge, 10 parts of red mud and 6 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 2:4:4. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 5:2:3.
The method comprises the following specific steps:
s1 grinding of raw materials
Drying oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag and red mud in an electrothermal blowing drying oven (105+/-5 ℃) to constant weight, weighing according to the parts by weight, putting the materials in an vertical stirring ball mill for mixed grinding for 1h, selecting corundum balls as grinding media, setting the rotation speed of a cylinder body to 300r/min and the rotation speed of a stirring shaft to 1000r/min, and then taking out the powder obtained through grinding and passing through a 0.075mm screen to obtain mixed raw materials;
s2 preparation of foaming agent microsphere
Placing the salt gypsum into a Buchner funnel paved with filter paper, and then adding water for leaching for 1min, so as to wash residual salt in the salt gypsum; putting the gypsum salt, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag into an electrothermal blowing drying oven (105+/-5 ℃) to be dried to constant weight for standby;
weighing the salt gypsum, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag according to the parts by weight, putting the materials into an vertical stirring ball mill, mixing and dry-grinding for 1h, selecting corundum balls as grinding media, and taking out the obtained powder after grinding is finished and passing through a 0.075mm screen for later use, wherein the rotating speed of a stirring shaft is 1000 r/min;
pouring the powder into a powerful mixer, adding atomized water, setting the rotating speed of a rotor of the powerful mixer to 1600r/min, setting the rotating speed of a cylinder to 40r/min, and stopping working after the powerful mixer rotates for 10min to obtain microspheres;
placing the microspheres in a vibrating screen, and sieving the microspheres for 5min through screens with the mesh numbers of 18 meshes (1.000 mm), 25 meshes (0.710 mm), 40 meshes (0.425 mm) and 60 meshes (0.250 mm) in sequence to obtain three foaming agent microspheres, wherein the particle sizes of the three foaming agent microspheres are respectively X1, X2 and X3, and X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm;
s3 preparation of oil-based rock debris hollow ceramsite green pellets
Forming the microspheres of foaming agents with different particle size specifications into gradations, wherein the weight part ratio of the microspheres of the foaming agents of X1, X2 and X3 is 2:4:4, adding 15+/-1% of water into the mixed raw material in the step S1 to mix to form a dough with a certain molding shape, then adopting a 12mm granulating plate to divide the dough into blocks, extruding and rolling to obtain a hollow ceramsite green body, and putting the hollow ceramsite green body into a blast drying box (105+/-5 ℃) to dry to constant weight to obtain a green body ball with the diameter of 11-13 mm;
s4, roasting and cooling step by step
Uniformly placing the green pellets in a muffle furnace paved with high-temperature ceramic fiber paper, and roasting by a step-by-step roasting method, wherein a firing system of the step-by-step roasting method comprises three stages, namely, the first stage is that the room temperature is raised to 500 ℃, the temperature is kept for 20min, and the heating rate is 10 ℃/min; the second stage is to raise the temperature to 950 ℃ at 500 ℃ and the heating rate is 10 ℃/min; the third stage is to raise the temperature to 1120 ℃ at 950 ℃ and keep the temperature at 1120 ℃ for 10min at a heating rate of 5 ℃/min, and then cool to room temperature by adopting a cooling mode along with the furnace, thus obtaining the hollow ultra-light ceramsite.
Example 2
In this example, in the dry state, the materials were weighed in parts by weight: 50 parts of oil-based rock debris residues, 25 parts of high-carbon ferrochrome slag, 15 parts of fluorine-containing sludge, 10 parts of red mud and 6 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 2:4:4. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 5:2:3.
The method comprises the following specific steps:
s1 grinding of raw materials
Drying oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag and red mud in an electrothermal blowing drying oven (105+/-5 ℃) to constant weight, weighing according to the parts by weight, putting the materials in an vertical stirring ball mill for mixed grinding for 1h, selecting corundum balls as grinding media, setting the rotation speed of a cylinder body to 300r/min and the rotation speed of a stirring shaft to 1000r/min, and then taking out the powder obtained through grinding and passing through a 0.075mm screen to obtain mixed raw materials;
s2, mixing the foaming agent and the mixed raw material with water to prepare a green ball; wherein the foaming agent is the existing material, and the common high-temperature foaming agent SiC is adopted.
S3, roasting the green pellets by adopting a step-by-step roasting method, and cooling to obtain hollow ultra-light ceramsite; the firing system of the step-by-step firing method comprises three stages, wherein the first stage is to heat up to 500 ℃ at room temperature and heat up for 20min at a heating rate of 10 ℃/min; the second stage is to raise the temperature to 950 ℃ at 500 ℃ and the heating rate is 10 ℃/min; the third stage is to raise the temperature to 1120 deg.C at 950 deg.C and keep the temperature at 1120 deg.C for 10min at a heating rate of 5 deg.C/min.
Example 3
On the basis of the embodiment 1, the materials are weighed according to the following parts by weight in a dry state: 50 parts of oil-based rock debris residues, 25 parts of high-carbon ferrochrome slag, 15 parts of fluorine-containing sludge, 10 parts of red mud and 6 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 2:4:4. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 5:2:3.
And in the step S4, uniformly placing the green pellets in a muffle furnace paved with high-temperature ceramic fiber paper, heating the green pellets to 1120 ℃ at a temperature of 5 ℃/min for 10min, and cooling the green pellets to the room temperature in a furnace cooling mode to obtain the hollow ultra-light ceramsite. The remaining steps were the same as in example 1.
Example 4
On the basis of example 1, in the dry state, the materials were weighed in parts by weight: 50 parts of oil-based rock debris residues, 25 parts of high-carbon ferrochrome slag, 15 parts of fluorine-containing sludge, 10 parts of red mud and 6 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 2:4:4. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 8:1:1. The specific preparation procedure was the same as in example 1.
Example 5
On the basis of example 1, in the dry state, the materials were weighed in parts by weight: 50 parts of oil-based rock debris residues, 25 parts of high-carbon ferrochrome slag, 15 parts of fluorine-containing sludge, 10 parts of red mud and 6 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 8:1:1. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 5:2:3. The specific preparation procedure was the same as in example 1.
Example 6
In a dry state, weighing the materials according to the following parts by weight: 30 parts of oil-based rock debris residues, 10 parts of high-carbon chromium iron slag, 30 parts of fluorine-containing sludge, 30 parts of red mud and 5 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 2:4:4. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 5:2:3. The specific preparation procedure was the same as in example 1.
Example 7
In a dry state, weighing the materials according to the following parts by weight: 45 parts of oil-based rock debris residues, 25 parts of high-carbon chromium iron slag, 20 parts of fluorine-containing sludge, 10 parts of red mud and 6 parts of foaming agent microspheres. The foaming agent microsphere comprises three kinds of particles with the particle diameters of X1, X2 and X3, wherein X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 1:4:5. The weight part ratio of the salt gypsum to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag in the foaming agent microspheres is 4:2:4.
In step S4, the third temperature was increased to 950 ℃ in the same manner as in example 1 except that the temperature was increased to 1150 ℃ in the same manner as in example 1.
Example 8
In a dry state, weighing the materials according to the following parts by weight: 55 parts of oil-based rock debris residues, 15 parts of high-carbon chromium iron residues, 10 parts of fluorine-containing sludge, 20 parts of red mud and 10 parts of foaming agent microspheres, wherein the foaming agent microspheres comprise three types of particles with the particle diameters of X1, X2 and X3, and X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the foaming agent microspheres of X1, X2 and X3 is 4:4:2, and the weight part ratio of the salt gypsum, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag in the foaming agent microspheres is 3:2:5. In step S4, the third stage was performed by raising the temperature of 950 ℃ to 1050 ℃ based on example 1, and the other steps were the same as the preparation steps of example 1.
Example 9
In a dry state, weighing the materials according to the following parts by weight: 45 parts of oil-based rock debris residues, 20 parts of high-carbon ferrochrome residues, 20 parts of fluorine-containing sludge, 15 parts of red mud and 8 parts of foaming agent microspheres, wherein the foaming agent microspheres comprise three types of particles with the particle diameters of X1, X2 and X3, and X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 4:2:4, and the weight part ratio of the salt gypsum, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag in the foaming agent microspheres is 4:1:5. In step S4, the third stage was performed by raising the temperature of 950 ℃ to 1120 ℃ based on example 1, and the other steps were the same as the preparation steps of example 1.
Example 10
In a dry state, weighing the materials according to the following parts by weight: 50 parts of oil-based rock debris residues, 20 parts of high-carbon ferrochrome residues, 15 parts of fluorine-containing sludge, 15 parts of red mud and 8 parts of foaming agent microspheres, wherein the foaming agent microspheres comprise three types of particles with the particle diameters of X1, X2 and X3, and X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm. The weight part ratio of the X1, X2 and X3 foaming agent microspheres is 3:3:4, and the weight part ratio of the salt gypsum, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag in the foaming agent microspheres is 5:1:4. In step S4, the third stage was performed by raising the temperature of 950 ℃ to 1080 ℃ based on example 1, and the other steps were the same as the preparation steps of example 1.
Experimental example 1
XRD analysis was performed on the hollow ultra-light ceramsite prepared in example 1 and examples 7-10, and the analysis results are shown in FIG. 1. The hollow ultra-light ceramsite in example 1 is subjected to acid corrosion, and then a crystal micro-morphology graph and an EDS energy spectrum of the hollow ultra-light ceramsite are obtained, as shown in fig. 2, wherein (a) is the crystal micro-morphology of the ceramsite subjected to acid corrosion; (b) EDS spectra of celsian crystals; (c) EDS spectrum of the heavy rock crystals. CT scan of the hollow ultralight ceramsite of example 1 was performed, and the CT scan is shown in fig. 3. CT scan of the hollow ultralight ceramsite of example 2 was performed, and the CT scan is shown in fig. 4.
As can be seen from FIGS. 1-3, the hollow ultra-light ceramsite phase prepared by the method is mainly composed of celsian, anorthite and forsterite, and contains mullite, quartz, hematite and other crystals. The hollow ultra-light ceramsite consists of a hollow inner core and a porous outer periphery, wherein the inner core of the hollow ultra-light ceramsite is in a hollow closed cavity structure and is in a sphere-like shape; the periphery is traditional porous ceramic structure, and it comprises a large amount of closed holes, and open hole quantity is few, has low water absorption characteristics simultaneously, and this hollow haydite structure is porous ceramic structure than traditional hollow haydite its periphery, has reduced the stress concentration phenomenon and open hole quantity when pressing and is few, and the water absorption is lower.
The hollow ceramsite with the application number of 201911283048.7, the preparation method thereof and the light hollow ceramsite with the application number of 201210462747.X are characterized in that the hollow ceramsite prepared by the preparation method is of a hollow structure, the outer layer is of a compact structure, the hollow ultra-light ceramsite prepared by the invention consists of a hollow inner core and the periphery of porous ceramic, and the raw materials are solid waste materials, so that the hollow ultra-light ceramsite has lower water absorption rate in terms of performance.
Experimental example 2
Reference GB/T17431.2-2010 "lightweight aggregate and test method section 2: light aggregate test method, the cylinder pressure strength, bulk density, 1h water absorption and porosity of the hollow ultra-light ceramsite prepared in examples 1-10 are measured, and are shown in Table 1;
TABLE 1
Carrying out heavy metal leaching concentration test on the mixed raw material in the step S1 of the example 1 and the hollow ultra-light ceramsite prepared in the example 1 to obtain a table 2;
TABLE 2
As can be seen from tables 1 and 2, the preparation methods of examples 1 and 7-10 and the hollow ultra-light ceramsite are all within the protection scope of the invention, and have low water absorption, the hollow ultra-light ceramsite cylinder pressure is 4-6MPa, and the bulk density is 400-500kg/m 3 The water absorption rate is 0.5-2%, the porosity is 55-65%, and meanwhile, the leaching values of heavy metal ions meet the limit requirements of GB 5985.3-2007 hazardous waste identification Standard leaching toxicity identification.
Example 2 was identical to example 1 in composition and preparation method, but the foaming agent used was the existing high temperature foaming agent material commonly used, example 1 was prepared by the preparation method of the present invention, example 2 also had lower water absorption and lower bulk density, but the bulk density and water absorption were higher than in example 1, and the hollow structure required in the present invention could not be obtained.
Example 3 in comparison with example 1, the step S4 of example 3 is not performed with the staged calcination, but the temperature is directly raised to 1120 ℃, the drum pressure strength of example 3 is lower than 4MPa and the water absorption is higher than 2%, and the calcination process also affects the formation of the hollow ultra-light ceramsite required by the present invention.
Example 4 compared with example 1, the weight parts of the gypsum salt and the ceramic polishing slag in example 4 are outside the protection scope of the invention; example 5 compared to example 1, the weight parts ratio of the three blowing agent microspheres is outside the scope of the present invention; example 6 in comparison with example 1, the weight parts of oil-based rock debris residues, high carbon ferrochrome slag, fluorine-containing sludge, red mud and foaming agent microspheres are outside the protection scope of the invention. The hollow ultralight ceramsite prepared in examples 4-6 has the characteristics that the liquid phase content, liquid phase viscosity, crystal structure, pore size and the like of the ceramsite are greatly changed in the high-temperature roasting process due to the differences of the components of the base material, the components of the foaming agent microspheres, the size and the like, so that the required requirements of the invention cannot be met, and the ceramic ceramsite has a bulk density of 400-500kg/m 3 In the case, the device also has high cylinder pressureStrength and low water absorption.
Therefore, the hollow ultra-light ceramsite prepared by the invention has the characteristics of small density, high strength and low water absorption, the sphere center of the ceramsite is of a closed cavity structure, the middle cavity and the outside are separated by a layer of porous ceramic structure, and the performance of the hollow ceramsite is superior to that of GB/T17431.1-2010 light aggregate and the test method part 1 thereof: the requirement of light aggregate, the leaching concentration of heavy metal is far lower than the limit requirement of GB 5052.3-2007 hazardous waste identification Standard leaching toxicity identification, the problems of high cost, complex preparation process, high environmental pollution risk and the like of the existing hollow ceramsite raw materials are solved, and a new way is provided for recycling the oil-based rock debris residues.
The foregoing description of the embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The preparation method of the hollow ultra-light ceramsite based on the oil-based rock debris is characterized by comprising the following steps of:
s1, grinding and mixing oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag and red mud to obtain mixed raw materials;
s2, mixing the foaming agent microspheres with the mixed raw material by adding water to prepare green pellets;
s3, roasting the green pellets by adopting a step-by-step roasting method, and cooling to obtain hollow ultra-light ceramsite; the firing system of the step firing method comprises three stages, wherein the first stage is to heat up to 400-600 ℃ at room temperature and keep the temperature for 10-30min; the second stage is to raise the temperature to 800-1000 ℃ at 400-600 ℃; the third stage is to raise the temperature of 800-1000 deg.C to 1050-1150 deg.C and keep the temperature at 1050-1150 deg.C for 5-20min.
2. The method for preparing the hollow ultra-light ceramsite based on the oil-based rock debris, as set forth in claim 1, wherein the foaming agent microsphere comprises the following preparation steps:
grinding and mixing the washed salt gypsum, the waste bamboo charcoal-based adsorbent and the ceramic polishing slag to obtain powder;
pouring the powder into a powerful mixer, adding atomized water, setting the rotating speed of a rotor of the powerful mixer to be 1200-2000r/min, setting the rotating speed of a cylinder to be 30-50r/min, and stopping working after the powerful mixer rotates for 5-15min to obtain microspheres;
the microspheres are placed in a vibrating screen and sequentially screened by screens with the mesh numbers of 18 meshes, 25 meshes, 40 meshes and 60 meshes to obtain three foaming agent microspheres, wherein the particle sizes of the three foaming agent microspheres are respectively X1, X2 and X3, and X1 is more than or equal to 0.710 and less than or equal to 1.000mm, X2 is more than or equal to 0.425 and less than or equal to 0.710mm, and X3 is more than or equal to 0.250 and less than or equal to 0.425mm.
3. The method for preparing the hollow ultra-light ceramsite based on the oil-based rock debris, which is disclosed in claim 2, is characterized in that in the step S2, the weight part ratio of the three foaming agent microspheres of X1, X2 and X3 is 0.5-4:2-4:2-6.
4. The method for preparing the hollow ultra-light ceramsite based on the oil-based rock debris, which is characterized in that in the step S2, three foaming agent microspheres are mixed with mixed raw materials by adding water, and a granulating plate with the diameter of 12mm is adopted to obtain a green ball with the diameter of 11-13mm through blocking, extrusion and rolling.
5. The preparation method of the hollow ultra-light ceramsite based on the oil-based rock debris, which is disclosed in claim 2, is characterized in that the weight ratio of the gypsum salt to the waste bamboo charcoal-based adsorbent to the ceramic polishing slag is 3-5:1-2:3-5.
6. The preparation method of the hollow ultra-light ceramsite based on the oil-based rock debris is characterized in that in the step S1, oil-based rock debris residues, fluorine-containing sludge, high-carbon chromium iron slag and red mud are dried, mixed and ground for 0.8-1.5h through a stirring ball mill, the rotation speed of a cylinder is 150-350r/min, the rotation speed of a stirring shaft is 900-1200r/min, and mixed raw materials are obtained through a screen of 0.075mm after grinding.
7. The preparation method of the hollow ultra-light ceramsite based on the oil-based rock debris, which is disclosed in claim 1, is characterized by comprising the following components in parts by weight in the steps S1 and S2: 40-60 parts of oil-based rock debris residues, 15-30 parts of high-carbon ferrochrome residues, 10-20 parts of fluorine-containing sludge, 10-20 parts of red mud and 6-10 parts of foaming agent microspheres.
8. The method for preparing the hollow ultra-light ceramsite based on the oil-based rock debris, which is characterized in that the heating rate of the first stage in the step S3 is 8-15 ℃/min; the temperature rising rate of the second stage is 8-15 ℃/min.
9. The method for preparing the hollow ultra-light ceramsite based on the oil-based rock debris, as set forth in claim 1, wherein the heating rate of the third stage in the step S3 is 5-10 ℃/min.
10. Hollow ultra-light ceramsite prepared by the preparation method according to any one of claims 1-9.
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