CN114988849B - Method for preparing high-strength ceramsite by using dried drilling mud as raw material - Google Patents
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Abstract
The invention provides a method for preparing high-strength ceramsite by using dried drilling mud as a raw material, wherein the method uses the dried drilling mud as a main raw material, prepares raw material powder with fluxing agent and strength additive in a certain proportion, and prepares the high-strength ceramsite after the procedures of grinding, crushing, granulating, multi-stage roasting, annealing treatment and the like, wherein the barrel pressure strength of the high-strength ceramsite can reach 90Mpa and above, and the method completely meets the requirements of building materials, oilfield underground propping agents and the like on strength.
Description
Technical Field
The invention relates to a preparation technology for high-strength ceramsite, in particular to a method for preparing high-strength ceramsite by using dried drilling mud as a raw material.
Background
The ceramsite is a kind of light aggregate produced by using inorganic material as main material and through the processes of pretreatment of the material, pelletizing, roasting, cooling, etc. The ceramsite is in a regular spherical shape or an elliptic spherical shape, the outer surface of the ceramsite is provided with a waterproof hard glaze shell, the inside of the ceramsite is provided with a closed micropore structure, and the ceramsite has excellent properties such as low density, high cylinder pressure intensity, high porosity, high softening coefficient and good freezing resistance and can be widely applied to the fields of fracturing oil extraction, high-rise buildings, fire resistance and heat preservation, road construction and the like.
According to the new standard of GB/T17431.1-1998 (light aggregate and test method thereof), the high-strength ceramsite refers to the light coarse aggregate for the structure, the strength grade of which is not less than 25 MPa. The technical requirements are that other indexes (particle size distribution, softening coefficient, particle type coefficient, harmful substance content and the like) are the same as those of the ultra-light common ceramsite except specific indexes of density grade, cylinder pressure strength, strength mark and water absorption. The traditional high-strength ceramsite mainly uses bauxite, kaolin and the like as raw materials, so that the consumption of resources is large, the production cost is high, and the market use of the materials is severely restricted. Therefore, in order to save the cost, more and more industrial production or biological treatment byproducts, solid waste and the like are used as raw materials to prepare the high-strength ceramsite.
Patent 110357651A discloses a method for preparing high-strength ceramsite by using dredging sludge of a Yunnan pond as a raw material, which comprises the following steps: step one: the dredging sludge of the Dian pond is subjected to sand removal treatment through a sieve with 100-200 meshes: step two: drying in an oven at a temperature of 80-105 ℃: step three: grinding the dried sludge by using a ball mill until the screen residue of 80 mu m is 10% -30%; step four:granulating into balls with the particle size of 5-20mm: step five: and (5) cooling to room temperature after high-temperature baking in a muffle furnace. The patent is prepared by using the dredging sludge of the Yunnan pond as a raw material, the water absorption rate of the finally obtained ceramsite is less than or equal to 8 percent, the barrel pressure strength is 7.8-18.6Mpa, and the bulk density is 800-1200kg/m 3 。
Patent CN107663099a discloses a high-strength ceramsite containing polluted soil and a preparation method thereof. The main raw materials adopted are fly ash, polluted soil and bentonite, the raw materials are mixed according to 60-80 parts of fly ash, 10-30 parts of polluted soil and 10 parts of bentonite, and the high-strength ceramsite prepared by pelleting, drying, roasting and cooling has the barrel pressure strength of 5-12 MPa and the water absorption rate of 2-14%.
Patent CN106904938A discloses a high-strength ceramsite taking coal gangue as raw material and fuel, which comprises the following raw material components in percentage by mass: 80-95% of gangue, 4.5-16% of feldspar, 0-5% of limestone and 0.1-0.5% of foaming agent; in addition, the preparation method comprises the steps of mixing the raw material components in proportion, grinding, balling, surface coating, drying, preheating, high-temperature sintering foaming, cooling and the like to prepare the high-strength ceramsite with the bulk density of 500-800 kg/m 3 The barrel pressure strength is 6-10 MPa, and the water absorption is less than 6%.
In summary, the problems in the prior art still remain that the ceramsite prepared by using solid waste such as fly ash or sludge as raw material cannot meet the requirement of high strength standard, and large-scale industrial production cannot be realized yet. In the oil field exploration process, the yield of drilling mud is huge, and the reduction treatment becomes a main means, but the treatment of the reduced drilling mud is not effectively solved. Although the dried drilling mud contains abundant aluminum, silicon, and other elements, the basic requirement for preparing the high-strength ceramsite is met, the quality of the raw materials cannot meet the requirement for preparing the high-strength ceramsite.
Therefore, development of a high-strength ceramsite and low-cost preparation process which can be applied to the related requirements of building materials and can meet the requirements of petroleum propping agents and the like on reaching higher strength standards is a technical problem to be solved.
Disclosure of Invention
The invention provides a method for preparing high-strength ceramsite by taking dried drilling mud as a main raw material, preparing raw material powder with fluxing agent and strength additive according to a certain proportion, and carrying out procedures such as grinding, crushing, granulating, multistage roasting, annealing treatment and the like to obtain the high-strength ceramsite, wherein the cylinder pressure strength is up to more than 90MPa, and the high-strength ceramsite can be used as building materials, underground propping agents of oil fields and the like, so that the technical problem that high-strength ceramsite can be produced by low-quality raw materials is solved, and the method has good industrial application prospect.
The technical scheme of the invention is as follows:
a method for preparing high-strength ceramsite, which comprises the following steps:
s1: raw material preparation: taking dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse powder with fineness of below 200 meshes, and then adding an intensity additive for secondary crushing to obtain raw material powder with fineness of not less than 600 meshes;
s2: extrusion, molding and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying an intensity solution on the raw material powder, extruding the raw material powder into granules after wetting, putting the granules into polishing equipment for polishing and forming, and finally, putting the granules into a closed space for aging at a temperature not lower than 25 ℃ to obtain raw ceramsite;
s3: three-stage sintering and solidifying: sequentially adopting low-temperature sintering, medium-temperature sintering and high-temperature sintering solidification to the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous ceramsite;
s4: annealing and cooling: and placing the obtained high-temperature homogeneous ceramsite into an annealing bin for stay annealing, and cooling in a natural environment to obtain the high-strength ceramsite.
Further, in step S1, the dried drilling mud includes the following components in mass fraction: 24.6-36.8% aluminum, 46.4-56.6% silicon, 12.8-22.4% calcium, based on the mass of the dry drilling mud.
Further, in step S1, the mass ratio of the dried drilling mud to the fluxing agent is 90-95:5-10.
Further, the fluxing agent comprises red mud and alkaline blast furnace slag, and the mass ratio of the red mud to the alkaline blast furnace slag is 2-3:1.
Further, in step S1, the mass ratio of the coarse grinding powder to the strength additive is 95-97:3-5.
Further, the strength additive comprises silicon carbide and aluminum oxide, wherein the mass ratio of the silicon carbide to the aluminum oxide is 3-4:1.
In step S1, the primary grinding is coarse grinding and the secondary grinding is fine grinding, each in a different manganese steel grade ball mill, which is conventional equipment well known to those skilled in the art.
In the step S1, the main purpose of adding the fluxing agent is to reduce the activation energy required by material melting in the subsequent high-temperature roasting stage by utilizing the characteristic of high alkalinity, so that the glassy melting point of the high-strength ceramsite is greatly reduced; the main purpose of adding the strength additive is to adjust the silicon-aluminum ratio of the dried drilling mud, and then the strength additive plays a role of a basic framework for molten materials in a high-temperature sintering process in an annealing treatment process.
Further, in step S2, the preparation method of the strength solution is as follows: and (3) regulating the sodium silicate solution with the concentration of 10% to a suspension by adopting sulfuric acid, so that the pH value of the suspension is 4.5-5.5, and the sodium silicate solution is based on the mass of the raw material powder.
Further, the strength solution is added in an amount of not more than 5%.
In step S2, sodium silicate (sodium silicate) in the strength solution is converted into gel-like silica gel in an acidic environment, so that not only an effective gluing effect is achieved on raw material powder, no additional binder is needed in the extrusion granulating process, but also the amorphous silica gel formed in the aging process can partially fill the internal pores of the granules, further, in the sintering process of step S3, the amorphous silica gel is molten in a glassy state, then forms high-temperature homogeneous ceramic particles with the main framework structure of the raw ceramic particles, and finally, in step S4, crystal quartz is formed through further crystallization in the annealing process to enhance the strength of the raw ceramic particles.
Further, in step S2, the polishing apparatus is a polishing apparatus with a plastic lining on an inner wall.
Further, in the step S3, the temperature of the low-temperature sintering is 300-450 ℃, and the low-temperature residence time is not less than 2 hours;
further, in the step S3, the temperature of the intermediate temperature sintering is 650-850 ℃, and the intermediate temperature residence time is not less than 2h.
Further, in the step S3, the high-temperature sintering temperature is 1050-1250 ℃, and the high-temperature residence time is not less than 2h.
Further, deep dehydration and organic matter inorganic carbonization of the raw ceramic particles are realized in the low-temperature sintering stage, so that gaseous substances are diffused and pores are formed in the raw ceramic particles, and the phenomenon that the subsequent strength is influenced due to the fact that the gaseous substances rush out of ceramic particle forming channels due to overhigh temperature is avoided; the intermediate-temperature sintering stage is used for carrying out glassy state melting of the amorphous silica gel and filling the internal pores of the raw ceramsite in the low-temperature sintering stage; and the high-temperature sintering stage is used for carrying out an integral melting and homogenizing process of a main framework structure and molten silica gel in the raw ceramic granules to form homogeneous ceramic granule framework components and silica gel filling components.
Further, in step S4, a recrystallization process is performed in the annealing stage, the molten silica gel formed in step S3 is primarily crystallized to form a crystal lattice, and after cooling, an integrated structure supported by the strength additive-crystal lattice and filled with amorphous silica gel is finally formed.
Further, in the annealing stage, the temperature of the annealing chamber is 700 to 800 ℃.
The invention has the following remarkable technical effects:
(1) The invention takes the dried drilling mud as the main raw material, and prepares reasonable auxiliary agent and preparation process for the specific raw material, so that the high-strength ceramsite can be produced by using low-quality raw material, and the requirements of building material specification and petroleum propping agent specification can be met simultaneously, and the invention has low cost, wide application range and good industrial application prospect;
(2) According to the preparation method, through a three-stage sintering process and a one-stage annealing design in the preparation stage, the raw materials and the auxiliary agent are subjected to specific reaction, the effect of obtaining the high-strength ceramsite by using the low-price raw materials is achieved by utilizing the mutual correspondence of the mechanism process of ceramsite strength formation and crystal production dynamics, and meanwhile, the preparation method has good operability and reproducibility.
Detailed Description
The invention is described in detail below with reference to examples:
preparation example 1
The preparation method of sample 1 is as follows:
s1: raw material preparation: taking dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse powder with fineness of below 200 meshes, and then adding an intensity additive for secondary crushing to obtain raw material powder with fineness of not less than 600 meshes; the dry drilling mud comprises the following components in percentage by mass: 24.6-36.8% aluminum, 46.4-56.6% silicon, 12.8-22.4% calcium, based on the mass of the dried drilling mud;
the mass ratio of the dried drilling mud to the fluxing agent is 93.5:6.5; the fluxing agent comprises red mud and alkaline blast furnace slag, and the mass ratio of the red mud to the alkaline blast furnace is 2.5:1;
the mass ratio of the coarse grinding powder to the strength additive is 96:4, a step of; the strength additive comprises silicon carbide and aluminum oxide, and the mass ratio of the silicon carbide to the aluminum oxide is 3.5:1;
s2: extrusion, molding and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying an intensity solution on the raw material powder, performing extrusion molding to obtain granules with the diameter of 1mm after wetting, putting the granules into polishing equipment for polishing and molding, and finally, putting the granules into a closed space for aging at the temperature of not lower than 25 ℃ to obtain raw ceramsite;
the preparation method of the strength solution comprises the following steps: adjusting the solution of the sodium silicate solution with the concentration of 10% to a suspension by adopting sulfuric acid, wherein the final pH value is 5, and the addition amount of the strength solution is 4.5% based on the mass of the raw material powder;
s3: three-stage sintering and solidifying: sequentially adopting low-temperature sintering, medium-temperature sintering and high-temperature sintering solidification to the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous ceramsite;
the low-temperature sintering temperature is 400 ℃, and the low-temperature residence time is 3 hours; the temperature of the intermediate temperature sintering is 800 ℃, and the intermediate temperature residence time is 3 hours; the high-temperature sintering temperature is 1200 ℃, and the high-temperature retention time is 3h.
S4: annealing and cooling: placing the obtained high-temperature homogeneous ceramsite into an annealing bin for stay annealing, and cooling in a natural environment to obtain high-strength ceramsite;
in the annealing stage, the temperature of the annealing bin is 750 ℃.
Preparation example 2
Sample 2 was prepared as follows:
s1: raw material preparation: taking dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse powder with fineness of below 200 meshes, and then adding an intensity additive for secondary crushing to obtain raw material powder with fineness of not less than 600 meshes; the dry drilling mud comprises the following components in percentage by mass: 24.6-36.8% aluminum, 46.4-56.6% silicon, 12.8-22.4% calcium, based on the mass of the dried drilling mud;
the mass ratio of the dried drilling mud to the fluxing agent is 90:10; the fluxing agent comprises red mud and alkaline blast furnace slag, and the mass ratio of the red mud to the alkaline blast furnace is 2:1;
the mass ratio of the coarse grinding powder to the strength additive is 95:5, a step of; the strength additive comprises silicon carbide and aluminum oxide, and the mass ratio of the silicon carbide to the aluminum oxide is 3:1;
s2: extrusion, molding and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying an intensity solution on the raw material powder, performing extrusion molding to obtain granules with the diameter of 1mm after wetting, putting the granules into polishing equipment for polishing and molding, and finally, putting the granules into a closed space for aging at the temperature of not lower than 25 ℃ to obtain raw ceramsite;
the preparation method of the strength solution comprises the following steps: adjusting the solution of the sodium silicate solution with the concentration of 10% to a suspension by adopting sulfuric acid, wherein the final pH value is 5, and the addition amount of the strength solution is 4.5% based on the mass of the raw material powder;
s3: three-stage sintering and solidifying: sequentially adopting low-temperature sintering, medium-temperature sintering and high-temperature sintering solidification to the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous ceramsite;
the low-temperature sintering temperature is 300 ℃, and the low-temperature residence time is 4 hours; the temperature of the intermediate temperature sintering is 850 ℃, and the intermediate temperature residence time is 3 hours; the high-temperature sintering temperature is 1150 ℃, and the high-temperature retention time is 3h.
S4: annealing and cooling: placing the obtained high-temperature homogeneous ceramsite in an annealing bin, and cooling in a natural environment to obtain high-strength ceramsite;
in the annealing stage, the temperature of the annealing bin is 700 ℃.
Preparation example 3
Sample 3 was prepared as follows:
s1: raw material preparation: taking dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse powder with fineness of below 200 meshes, and then adding an intensity additive for secondary crushing to obtain raw material powder with fineness of not less than 600 meshes; the dry drilling mud comprises the following components in percentage by mass: 24.6-36.8% aluminum, 46.4-56.6% silicon, 12.8-22.4% calcium, based on the mass of the dried drilling mud;
the mass ratio of the dried drilling mud to the fluxing agent is 95:5, a step of; the fluxing agent comprises red mud and alkaline blast furnace slag, and the mass ratio of the red mud to the alkaline blast furnace is 3:1;
the mass ratio of the coarse grinding powder to the strength additive is 97:3, a step of; the strength additive comprises silicon carbide and aluminum oxide, and the mass ratio of the silicon carbide to the aluminum oxide is 4:1;
s2: extrusion, molding and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying an intensity solution on the raw material powder, performing extrusion molding to obtain granules with the diameter of 1mm after wetting, putting the granules into polishing equipment for polishing and molding, and finally, putting the granules into a closed space for aging at the temperature of not lower than 25 ℃ to obtain raw ceramsite;
the preparation method of the strength solution comprises the following steps: adjusting the solution of the sodium silicate solution with the concentration of 10% to a suspension by adopting sulfuric acid, wherein the final pH value is 5.5, and the addition amount of the strength solution is 5.5% based on the mass of the raw material powder;
s3: three-stage sintering and solidifying: sequentially adopting low-temperature sintering, medium-temperature sintering and high-temperature sintering solidification to the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous ceramsite;
the temperature of the low-temperature sintering is 450 ℃, and the low-temperature residence time is 3 hours; the temperature of the intermediate temperature sintering is 700 ℃, and the intermediate temperature residence time is 4 hours; the high-temperature sintering temperature is 1200 ℃, and the high-temperature retention time is 3h.
S4: annealing and cooling: placing the obtained high-temperature homogeneous ceramsite into an annealing bin for stay annealing, and cooling in a natural environment to obtain high-strength ceramsite;
in the annealing stage, the temperature of the annealing bin is 750 ℃.
Test examples
According to the standard of GB/T17431.1-2010 (lightweight aggregate and test method thereof), the cylinder pressure intensity of the high-strength ceramsite of the sample 1 is 92.34Mpa, the cylinder pressure intensity of the high-strength ceramsite of the sample 2 is 98.64Mpa, and the cylinder pressure intensity of the high-strength ceramsite of the sample 3 is 102.68Mpa, which all meet the requirements of sand control propping agents and general-grade fracturing propping agents of oil fields;
according to GB/T50081-2002 of test method Standard for mechanical Properties of common concrete, the high-strength ceramsite prepared by sample 1 is mixed with common C30 Cement to prepare a standard concrete block, and the compressive strength of the concrete block is tested after curing for 28 days, and reaches 78.5Mpa, thus meeting the requirement of bearing concrete blocks.
The above description is only of the preferred embodiment of the present invention, and is not intended to limit the present invention in any other way, but is intended to cover any modifications or equivalent variations according to the technical spirit of the present invention, which fall within the scope of the present invention as defined by the appended claims.
Claims (2)
1. The method for preparing the high-strength ceramsite by using the dried drilling mud as the raw material is characterized by comprising the following steps of:
s1: raw material preparation: taking dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse powder with fineness of below 200 meshes, and then adding an intensity additive for secondary crushing to obtain raw material powder with fineness of not less than 600 meshes; the dry drilling mud comprises the following components in percentage by mass: 24.6-36.8% aluminum, 46.4-56.6% silicon, 12.8-22.4% calcium, based on the mass of the dried drilling mud;
the fluxing agent comprises red mud and alkaline blast furnace slag, and the mass ratio of the red mud to the alkaline blast furnace is 2-3:1;
the strength additive comprises silicon carbide and aluminum oxide, wherein the mass ratio of the silicon carbide to the aluminum oxide is 3-4:1;
the mass ratio of the coarse grinding powder to the strength additive is 95-97:3-5;
s2: extrusion, molding and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying an intensity solution on the raw material powder, extruding the raw material powder into granules after wetting, putting the granules into polishing equipment for polishing and forming, and finally, putting the granules into a closed space for aging at a temperature not lower than 25 ℃ to obtain raw ceramsite;
the preparation method of the strength solution comprises the following steps: adjusting the sodium silicate solution with the concentration of 10% to a suspension by adopting sulfuric acid, so that the pH value of the suspension is 4.5-5.5;
s3: three-stage sintering and solidifying: sequentially adopting low-temperature sintering, medium-temperature sintering and high-temperature sintering solidification to the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous ceramsite; the temperature of the low-temperature sintering is 300-450 ℃, and the low-temperature residence time is not less than 2 hours; the temperature of the intermediate temperature sintering is 650-850 ℃, and the intermediate temperature residence time is not less than 2h; the high-temperature sintering temperature is 1050-1250 ℃, and the high-temperature residence time is not less than 2h;
s4: annealing and cooling: and placing the obtained high-temperature homogeneous ceramsite into an annealing bin for stay annealing, and cooling in a natural environment to obtain the high-strength ceramsite.
2. The method of claim 1, wherein in step S1 the mass ratio of the dry drilling mud to the fluxing agent is 90-95:5-10.
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