CN114988849A - Method for preparing high-strength ceramsite by using dried drilling mud as raw material - Google Patents

Method for preparing high-strength ceramsite by using dried drilling mud as raw material Download PDF

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CN114988849A
CN114988849A CN202110223096.8A CN202110223096A CN114988849A CN 114988849 A CN114988849 A CN 114988849A CN 202110223096 A CN202110223096 A CN 202110223096A CN 114988849 A CN114988849 A CN 114988849A
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temperature
ceramsite
strength
raw material
drilling mud
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CN114988849B (en
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王晓慧
齐光峰
齐静静
赵金刚
范路
修长军
王韧
王伟斌
王芫芫
时宪
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China Petroleum and Chemical Corp
Technology Inspection Center of Sinopec Shengli Oilfield Co
Shengli Oilfield Testing and Evaluation Research Co Ltd
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China Petroleum and Chemical Corp
Technology Inspection Center of Sinopec Shengli Oilfield Co
Shengli Oilfield Testing and Evaluation Research Co Ltd
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Abstract

The invention provides a method for preparing high-strength ceramsite by using dried drilling mud as a raw material, which comprises the steps of preparing raw material powder by using the dried drilling mud as a main raw material, a fluxing agent and a strength additive according to a certain proportion, grinding, crushing, granulating, roasting at multiple stages, annealing and the like to obtain the high-strength ceramsite, wherein the cylinder pressure strength of the high-strength ceramsite can reach 90Mpa or more, and the high-strength ceramsite completely meets the requirements of building materials, oilfield downhole propping agents and the like on strength.

Description

Method for preparing high-strength ceramsite by using dried drilling mud as raw material
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 commonly known as artificial light aggregate, and is produced by using inorganic materials as main raw materials through the processes of raw material pretreatment, granulation, roasting, cooling and the like. The ceramsite is regular spherical or ellipsoidal, the outer surface of the ceramsite is provided with a waterproof hard glaze layer shell, the ceramsite is internally provided with a closed microporous structure, and the ceramsite has excellent properties such as low density, high cylinder pressure strength, 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, heat preservation, road construction and the like.
According to the new GB/T17431.1-1998 standard (light aggregate and test method thereof), the high-strength ceramsite is the structural light coarse aggregate with the strength index of not less than 25 MPa. The technical requirements are that the indexes (grain composition, softening coefficient, grain type coefficient, harmful substance content and the like) are the same as those of the ultra-light and ordinary ceramsite except that the density grade, the cylinder pressure strength, the strength grade and the water absorption rate have specific indexes. The traditional high-strength ceramsite mainly takes bauxite, kaolin and the like as raw materials, so that the consumption of resources is high, the production cost is high, and the market use of the materials is severely restricted. Therefore, in order to save cost, more and more by-products of industrial production or biological treatment, solid wastes 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 taking yunnan pond dredging sludge as a raw material, which comprises the following steps: the method comprises the following steps: the dredging sludge of the yunnan pond is subjected to desanding treatment through a 100-plus-200-mesh sieve: step two: drying in an oven at a temperature of 80-105 ℃: step three: grinding the dried sludge to 80 mu m with 10-30% of screen residue by using a ball mill; step four: pelletizing and granulating, wherein the particle size is 5-20 mm: step five: and (4) carrying out high-temperature roasting in a muffle furnace, and cooling to room temperature. The method is characterized in that the method completely utilizes the Dianchi lake dredging sludge as the raw material to prepare the ceramsite, the water absorption of the finally obtained ceramsite is less than or equal to 8 percent, the cylinder pressure strength is 7.8-18.6Mpa, and the bulk density is 800-1200 kg/m- 3
Patent CN107663099A discloses a high-strength ceramsite containing contaminated soil and a preparation method thereof. The main raw materials adopted by the method comprise 60-80 parts of fly ash, 10-30 parts of polluted soil and 10 parts of bentonite, and the raw materials are mixed according to the proportion of 60-80 parts of fly ash, 10-30 parts of polluted soil and 10 parts of bentonite, and the high-strength ceramsite prepared by granulating, drying, roasting and cooling has the cylinder pressure strength of 5-12 MPa and the water absorption rate of 2-14%.
Patent CN106904938A discloses a high-strength ceramsite using coal gangue as raw material and fuel, which comprises the following raw material components by mass percent: 80-95% of coal 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, and performing the processes of grinding, balling, surface coating, drying, preheating, high-temperature sintering foaming, cooling and the like to prepare the high-strength ceramsite, wherein the bulk density of the ceramsite is 500-800 kg/m 3 The cylinder pressure strength is 6-10 MPa, and the water absorption rate 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 can not meet the requirement of high strength standard, and the large-scale industrial production can not be realized. In the oil field exploration process, the yield of drilling mud is huge, and reduction treatment becomes a main means, but the treatment of the drilling mud after reduction is not effectively solved. Although the dried drilling mud contains rich elements such as aluminum, silicon and the like which have the basic requirements for preparing the high-strength ceramsite, the quality of the raw materials cannot meet the requirements for preparing the high-strength ceramsite.
Therefore, it is an urgent technical problem to develop a high-strength ceramsite and a low-cost preparation process which can be applied to the relevant requirements of building materials and can meet the requirements of petroleum proppants and the like to reach higher strength standards.
Disclosure of Invention
The invention provides a high-strength ceramsite which is prepared by taking dried drilling mud as a main raw material, mixing the dried drilling mud with a fluxing agent and a strength additive in a certain proportion, grinding, crushing, granulating, roasting in multiple stages, annealing and the like, wherein the cylinder pressure strength is higher than 90MPa, the high-strength ceramsite can be used as a building material, an oil field downhole propping agent and the like, the technical problem that the high-strength ceramsite can be produced from low-quality raw materials is solved, and the high-strength ceramsite has a good industrial application prospect.
The technical scheme of the invention is as follows:
a preparation method of high-strength ceramsite comprises the following steps:
s1: preparing raw materials: taking the dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse ground powder with the fineness of less than 200 meshes, and then adding a strength additive for secondary crushing to obtain raw powder with the fineness of not less than 600 meshes;
s2: extruding, forming and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying a strength solution to the raw material powder, wetting the raw material powder, extruding the raw material powder into granules, putting the granules into polishing equipment, performing round throwing molding, and finally, putting the granules into a closed space, and aging at a temperature of not lower than 25 ℃ to obtain raw ceramsite;
s3: three-stage sintering and curing: sequentially carrying out low-temperature sintering, medium-temperature sintering and high-temperature sintering curing on the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous-phase ceramsite;
s4: annealing and cooling: and placing the obtained high-temperature homogeneous-phase ceramsite in an annealing bin, standing for annealing, and keeping the high-temperature homogeneous-phase ceramsite in a natural environment for cooling to obtain the high-strength ceramsite.
Further, in step S1, the dried drilling mud includes the following components 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.
Further, in step S1, the mass ratio of the dried drilling mud to the flux 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 ground powder to the strength additive is 95-97: 3-5.
Further, the strength additive comprises silicon carbide and aluminum oxide, and 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 fluxing agent is added for the main purpose of reducing the activation energy required by material melting in the subsequent high-temperature roasting stage by utilizing the characteristic of high alkalinity of the fluxing agent, so that the glass melting point of the high-strength ceramsite is greatly reduced; the strength additive is added to adjust the silicon-aluminum ratio of the dried drilling mud, and provides a basic skeleton effect for molten materials in a high-temperature sintering process in an annealing treatment process.
Further, in step S2, the strength solution is prepared as follows: adjusting 10% sodium silicate solution to obtain suspension with pH of 4.5-5.5 based on the mass of the raw powder by using sulfuric acid.
Further, the strength solution is added in an amount of not more than 5%.
In step S2, sodium silicate in the strength solution is converted into gel-like silica gel in an acidic environment, which not only effectively adheres the raw material powder, so that no additional binder is required to be added in the extrusion granulation process, but also partially fills the internal pores of the granules with amorphous silica gel formed in the aging process, further, in the sintering process of step S3, the amorphous silica gel undergoes glass-state melting, then forms high-temperature homogeneous ceramsite with the main body framework structure of the raw ceramsite, and finally forms crystalline quartz through further crystallization in the annealing process of step S4 to enhance the strength of the raw ceramsite.
Further, in step S2, the polishing apparatus is a polishing apparatus with plastic-lined inner wall.
Further, in step S3, the temperature of the low-temperature sintering is 300-450 ℃, and the low-temperature retention time is not less than 2 h;
further, in step S3, the temperature of the medium-temperature sintering is 650-850 ℃, and the medium-temperature residence time is not less than 2 h.
Further, in step S3, the temperature of the high-temperature sintering is 1050-1250 ℃, and the high-temperature retention time is not less than 2 h.
Furthermore, the deep dehydration and organic matter inorganic carbonization of the raw ceramsite are realized in the low-temperature sintering stage, so that gaseous substances are diffused and pores are formed in the raw ceramsite, and the condition that the subsequent strength formation is influenced because the gaseous substances are rushed out of the ceramsite to form pore channels due to overhigh temperature is avoided; the intermediate-temperature sintering stage carries out glass state melting of the amorphous silica gel and is used for filling the pores inside the raw ceramsite in the low-temperature sintering stage; and in the high-temperature sintering stage, the integral melting and homogenizing process of the main body framework structure and the molten silica gel in the raw ceramsite is carried out, so that homogeneous ceramsite framework components and homogeneous silica gel filling components are formed.
Further, in step S4, a recrystallization process is performed in an annealing stage, the molten silica gel formed in step S3 is primarily crystallized to form a crystalline lattice, and a monolithic structure supported by a strength additive-crystalline lattice and filled with an amorphous silica gel is finally formed after cooling.
Further, in the annealing stage, the temperature of the annealing bin 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 utilizing the low-quality raw material, the standard requirement of building materials and the standard requirement of petroleum propping agents can be simultaneously met, the cost is low, the application range is wide, and the invention has good industrial application prospect;
(2) the preparation method of the invention realizes the effect of obtaining high-strength ceramsite by using low-price raw materials through a specific reaction between the raw materials and the auxiliary agents through a three-stage sintering process and a one-stage annealing design in the preparation stage and utilizing the mechanism process of ceramsite strength formation and the kinetics of crystal generation to correspond to each other.
Detailed Description
The invention is illustrated in detail below with reference to examples:
preparation example 1
Sample 1 was prepared as follows:
s1: preparing raw materials: taking the dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse ground powder with the fineness of less than 200 meshes, and then adding a strength additive for secondary crushing to obtain raw powder with the fineness of not less than 600 meshes; the dried 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 dry 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 slag is 2.5: 1;
the mass ratio of the coarse grinding powder to the strength additive is 96: 4; 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: extruding, forming and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying a strength solution on the raw material powder, wetting the raw material powder, extruding the raw material powder into granules with the diameter of 1mm, putting the granules into polishing equipment, performing round polishing molding, and finally, putting the granules into a closed space, and aging the granules at a temperature of not lower than 25 ℃ to obtain raw ceramsite;
the preparation method of the strength solution comprises the following steps: adjusting a 10% sodium silicate solution to a suspension by using sulfuric acid, wherein the final pH 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 curing: sequentially carrying out low-temperature sintering, medium-temperature sintering and high-temperature sintering curing on the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous-phase ceramsite;
the low-temperature sintering temperature is 400 ℃, and the low-temperature retention time is 3 hours; the temperature of the medium-temperature sintering is 800 ℃, and the medium-temperature retention time is 3 h; the high-temperature sintering temperature is 1200 ℃, and the high-temperature retention time is 3 h.
S4: annealing and cooling: placing the obtained high-temperature homogeneous-phase ceramsite in an annealing bin, staying for annealing, and keeping the high-temperature homogeneous-phase ceramsite in a natural environment for cooling 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: preparing raw materials: taking the dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse ground powder with the fineness of less than 200 meshes, and then adding a strength additive for secondary crushing to obtain raw powder with the fineness of not less than 600 meshes; the dried 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 slag is 2: 1;
the mass ratio of the coarse grinding powder to the strength additive is 95: 5; 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: extruding, forming and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying a strength solution on the raw material powder, wetting the raw material powder, extruding the raw material powder into granules with the diameter of 1mm, putting the granules into polishing equipment, performing round polishing and forming, and finally, putting the granules into a closed space, and 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 a 10% sodium silicate solution to a suspension by using sulfuric acid, wherein the final pH 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 curing: sequentially carrying out low-temperature sintering, medium-temperature sintering and high-temperature sintering curing on the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous-phase ceramsite;
the low-temperature sintering temperature is 300 ℃, and the low-temperature retention time is 4 hours; the temperature of the medium-temperature sintering is 850 ℃, and the medium-temperature retention time is 3 h; the temperature of the high-temperature sintering is 1150 ℃, and the high-temperature retention time is 3 h.
S4: annealing and cooling: placing the obtained high-temperature homogeneous-phase ceramsite in an annealing bin, keeping the high-temperature homogeneous-phase ceramsite in a natural environment, and cooling 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: preparing raw materials: taking the dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse ground powder with the fineness of less than 200 meshes, and then adding a strength additive for secondary crushing to obtain raw powder with the fineness of not less than 600 meshes; the dried 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; 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 3: 1;
the mass ratio of the coarse grinding powder to the strength additive is 97: 3; 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: extruding, forming and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying a strength solution on the raw material powder, wetting the raw material powder, extruding the raw material powder into granules with the diameter of 1mm, putting the granules into polishing equipment, performing round polishing and forming, and finally, putting the granules into a closed space, and aging at the temperature of not lower than 25 ℃ to obtain raw ceramsite;
the strength solution is prepared as follows: adjusting a 10% sodium silicate solution to a suspension by using sulfuric acid, wherein the final pH 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 curing: sequentially carrying out low-temperature sintering, medium-temperature sintering and high-temperature sintering curing on the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous ceramsite;
the low-temperature sintering temperature is 450 ℃, and the low-temperature retention time is 3 hours; the temperature of the medium-temperature sintering is 700 ℃, and the medium-temperature retention time is 4 h; the high-temperature sintering temperature is 1200 ℃, and the high-temperature retention time is 3 h.
S4: annealing and cooling: placing the obtained high-temperature homogeneous-phase ceramsite in an annealing bin, staying for annealing, and keeping the high-temperature homogeneous-phase ceramsite in a natural environment for cooling 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 (light aggregate and test method thereof), through tests, the cylinder pressure strength of the high-strength ceramsite of the sample 1 is 92.34Mpa, the cylinder pressure strength of the high-strength ceramsite of the sample 2 is 98.64Mpa, and the cylinder pressure strength 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 the standard GB/T50081-2002 of the mechanical property test method of the common concrete, the high-strength ceramsite prepared by the sample 1 is mixed with the common C30 cement to prepare a standard concrete block, the standard concrete block is cured for 28 days, and then the compressive strength of the standard concrete block is tested, wherein the compressive strength of the concrete block reaches 78.5Mpa, and the requirement of a load-bearing concrete block is met.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, but any modifications or equivalent variations made according to the technical spirit of the present invention are within the scope of the present invention as claimed.

Claims (10)

1. A method for preparing high-strength ceramsite by using dried drilling mud as a raw material is characterized by comprising the following steps:
s1: preparing raw materials: taking the dried drilling mud as a main raw material, adding a fluxing agent in the crushing process for primary crushing to obtain coarse ground powder with the fineness of less than 200 meshes, and then adding a strength additive for secondary crushing to obtain raw powder with the fineness of not less than 600 meshes;
s2: extruding, forming and aging: putting the raw material powder obtained in the step S1 into a double-roller extruder, spraying a strength solution to the raw material powder, wetting the raw material powder, extruding the raw material powder into granules, putting the granules into polishing equipment, performing round throwing molding, and finally, putting the granules into a closed space, and aging at a temperature of not lower than 25 ℃ to obtain raw ceramsite;
s3: three-stage sintering and curing: sequentially carrying out low-temperature sintering, medium-temperature sintering and high-temperature sintering curing on the raw ceramsite in an anoxic environment to obtain high-temperature homogeneous-phase ceramsite;
s4: annealing and cooling: and placing the obtained high-temperature homogeneous-phase ceramsite in an annealing bin, standing for annealing, and keeping the high-temperature homogeneous-phase ceramsite in a natural environment for cooling to obtain the high-strength ceramsite.
2. The method of claim 1, wherein in step S1, the dried drilling mud comprises the following components in percentage by mass: 24.6-36.8% of aluminum, 46.4-56.6% of silicon, and 12.8-22.4% of calcium, based on the mass of the dried drilling mud.
3. The method of claim 2, wherein in step S1, the mass ratio of the dried drilling mud to the flux is 90-95: 5-10.
4. The method according to claim 3, wherein 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.
5. The method of claim 1, wherein in step S1, the mass ratio of the coarse powder abrasive to the strength additive is 95-97: 3-5.
6. The method of claim 5, wherein the strength additive comprises silicon carbide and aluminum oxide in a mass ratio of 3-4: 1.
7. The method of claim 1, wherein in step S2, the strength solution is prepared by: adjusting 10% sodium silicate solution with sulfuric acid to obtain suspension with pH of 4.5-5.5.
8. The method as claimed in claim 1, wherein in step S3, the temperature of the low-temperature sintering is 300-450 ℃, and the low-temperature retention time is not less than 2 h.
9. The method as claimed in claim 8, wherein in step S3, the medium-temperature sintering temperature is 650-850 ℃, and the medium-temperature retention time is not less than 2 h.
10. The method as claimed in claim 9, wherein in step S3, the temperature of the high-temperature sintering is 1050-1250 ℃, and the high-temperature retention time is not less than 2 h.
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