WO2014172955A1 - 一种粉煤灰制石油压裂支撑剂及其制备方法 - Google Patents

一种粉煤灰制石油压裂支撑剂及其制备方法 Download PDF

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WO2014172955A1
WO2014172955A1 PCT/CN2013/076385 CN2013076385W WO2014172955A1 WO 2014172955 A1 WO2014172955 A1 WO 2014172955A1 CN 2013076385 W CN2013076385 W CN 2013076385W WO 2014172955 A1 WO2014172955 A1 WO 2014172955A1
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fly ash
powder
petroleum fracturing
fracturing proppant
mixture
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English (en)
French (fr)
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张胜杰
张林群
王英军
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鹤壁天瑞石油支撑剂有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B33/135—Combustion residues, e.g. fly ash, incineration waste
    • C04B33/1352—Fuel ashes, e.g. fly ash
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C04B2235/3267—MnO2
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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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
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
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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
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Definitions

  • the invention belongs to the technical field of petroleum fracturing proppants, and particularly relates to a petroleum fracturing proppant made of fly ash and a preparation method thereof. Background technique
  • fracturing In oil and gas oilfield exploitation, fracturing is widely used to increase oil well production, prolong the high-yield life of oil wells, and exploit difficult resources.
  • the proppant In order to prevent the closure of underground pressure cracks, retain the oil and gas channels, and maintain the conductivity, the proppant must be used to fill the cracks. Due to the different depth of the oil layer, the oily viscosity is different, and the properties of the proppant such as strength, apparent density and particle size are also different.
  • the fracturing support is divided into three categories: high density, high strength, medium density high strength and low density high strength. In recent years, there has been a demand for ultra low density of proppant.
  • the common particle size of fracturing proppants on the market is 16 ⁇ 30 mesh (1180 ⁇ 600 ⁇ ), 20 ⁇ 40 mesh (850 ⁇ 425 ⁇ ), 30 ⁇ 50 mesh (600 ⁇ 300 ⁇ ), 40-60 mesh (425 ⁇ 250 ⁇ ).
  • a variety of specifications, such as 40 ⁇ 70 mesh (425 ⁇ 212 ⁇ ) regardless of the type and specification, the petroleum fracturing proppant should have a low apparent density under the premise of sufficient crush resistance. Reduce the cost of fracturing, ensure the saturation of the pressure crack filling, and increase the oil well production.
  • the production of petroleum fracturing proppants is generally based on high alumina bauxite, supplemented by one or several metal oxides as mineralizers, such as manganese oxide, calcium oxide, iron oxide, magnesium oxide, zircon and the like.
  • the raw materials are pulverized, mixed, spheronized, and sintered to obtain a fracturing proppant.
  • the fracturing proppant disclosed in Chinese Patent No. 93111983.9 the main material is 70% ⁇ 90% of the cooked bauxite after being calcined and pulverized, and then the multi-component oxide and the soft clay are used to co-mill and Add water or organic solvent, then loosen, spheronize, sieving, sintering, polishing and re-screening.
  • a fracturing proppant is obtained.
  • the fracturing proppant disclosed in Chinese Patent Application No. 02157202.X is prepared by: 90% ⁇ 94% high grade raw bauxite, plus 6% ⁇ 10% manganese oxide ore powder, after 1330 °C ⁇ It is fired at a high temperature of 1350 °C.
  • 02157202.X is currently widely used in the production of proppant, but the fracturing proppant provided by this patent relies on special bauxite or first-grade bauxite and Mn0 2 with a content of more than 50%. High-quality resources such as manganese ore are prepared at higher temperatures. Therefore, high energy consumption and high resource consumption during the preparation process limit the further development of fracturing proppants. Summary of the invention
  • the technical problem to be solved by the present invention is to provide a fly ash petroleum fracturing proppant and a preparation method thereof, and the invention adopts low-cost fly ash as a raw material and is prepared at a lower temperature.
  • Petroleum fracturing proppants have low apparent density, strong crush resistance, and low cost, reducing energy consumption.
  • the invention provides a fly ash petroleum fracturing proppant, which is prepared from the following components: lwt% ⁇ 60wt% fly ash;
  • the balance is bauxite powder.
  • the petroleum fracturing proppant further comprises 0 wt% to 5 wt% of manganese ore powder.
  • Mn0 2 in the manganese ore powder accounts for 0 wt% to 5 wt% of the fly ash petroleum fracturing proppant.
  • the bauxite powder has an aluminum content of 35 wt% to 75 wt%.
  • the petroleum fracturing proppant has a bulk density of ⁇ 1.60 g/cm 3 and an apparent density of ⁇ 2.70 g/cm 3 .
  • the invention also provides a preparation method of a fly ash petroleum fracturing proppant, comprising the following steps:
  • the preparation method is: a) mixing fly ash, manganese ore powder, potassium feldspar powder and bauxite powder, homogenizing and refining treatment, granulating and sieving to obtain a mixture;
  • the mixture has a particle size of from 3,350 to 106 ⁇ m.
  • the step a) is specifically:
  • the fly ash, potassium feldspar powder, manganese ore powder and bauxite powder are mixed, placed in a forced mixer for homogenization and refining treatment, and after granulation, sieved to obtain a mixture.
  • the firing time is 4-8 hours.
  • the invention prepares a fly ash petroleum fracturing proppant by using fly ash, potassium feldspar powder and bauxite powder as raw materials, and the invention uses low-cost fly ash as raw material.
  • A1 2 0 3 in the fly ash generates mullite, and the surplus SiO 2 in the raw material is converted into a low-viscosity mineral such as phosphorus quartz, which reduces the apparent density of the product.
  • the invention provides a fly ash petroleum fracturing proppant, which is prepared from the following components: lwt% ⁇ 60wt% fly ash;
  • the balance is bauxite powder.
  • the invention uses fly ash as the main raw material of the petroleum fracturing proppant, and the fly ash is industrial waste, and the cost is low. Therefore, the rational use of the fly ash has the important significance of energy saving, environmental protection and resource conservation.
  • the mass of the fly ash in the total amount of the raw materials is preferably from 1% by weight to 60% by weight, more preferably 30 wt% to 55 wt%, most preferably 40 wt% to 50 wt%.
  • the K-feldspar powder is a mineralizer for a petroleum fracturing proppant, wherein K 2 0 in the K-feldspar powder acts as a mineralization.
  • the potassium feldspar powder is preferably added in an amount of from 1% by weight to 30% by weight, more preferably from 10% by weight to 25% by weight, most preferably from 15% by weight to 20% by weight, based on the total amount of the raw materials.
  • the content of A1 2 0 3 and Si0 2 in the raw material after mixing is adjusted by using bauxite powder, and the aluminum content in the bauxite powder is 35 wt% to 75 wt%, more preferably 50 wt% to 70 wt%.
  • the bauxite is preferably a tertiary alumina bauxite or a cooked bauxite, more preferably a tertiary alumina bauxite.
  • the raw material of the petroleum fracturing proppant prepared by the invention further comprises manganese ore powder, the manganese ore powder is an auxiliary mineralizer and a coloring agent, and Mn0 2 in the manganese ore powder accounts for the petroleum fracturing proppant of the fly ash. 0wt% ⁇ 5wt%.
  • the manganese ore fines are preferably added in an amount of from 0% by weight to 5% by weight based on the total amount of the raw materials, more preferably from 1% by weight to 4% by weight, most preferably from 2% by weight to 3% by weight.
  • the composite mineralizer formed by K 2 0 in potassium feldspar powder and Mn0 2 in manganese ore powder forms a liquid phase which accounts for 30% to 40% of the total volume of the raw materials in the raw materials mixed at a high temperature, and the resulting liquid Not only the surface tension is large, the wetting performance is good, the material is denser, and therefore, the strength of the petroleum fracturing proppant is increased.
  • the petroleum fracturing proppant provided by the present invention has a bulk density of ⁇ 1.60 g/cm 3 and an apparent density of ⁇ 2.70 g/cm 3 .
  • the bulk density is ⁇ 1.58 g/cm 3 and the apparent density is ⁇ 2.60 g/cm 3 .
  • the invention also provides a preparation method of a fly ash petroleum fracturing proppant, comprising the following steps:
  • the invention firstly mixes the fly ash, the potassium feldspar powder and the bauxite powder, and performs the homogenization and refinement treatment, and the manner of the homogenization refining treatment is not particularly limited, and the specific method is:
  • the fly ash, potassium feldspar powder and bauxite powder are placed in a forced mixer for homogenization and refining treatment.
  • the invention carries out the homogenization and refinement treatment of the raw materials, so that the particle size distribution of the raw materials is more uniform, the chemical reaction is more smooth, and the chemical reaction is carried out more fully, so that the grain of the petroleum fracturing proppant is finer and the oil fracturing is improved.
  • the strength of the proppant The fly ash, potassium feldspar powder and bauxite powder are placed in a forced mixer for homogenization and refining treatment, and after granulation, they are sieved to obtain a mixture.
  • the granulation method of the present invention is not particularly limited, and the granulation method well known to those skilled in the art may be used; the manner of sieving in the present invention is not particularly limited, and the sieving method well known to those skilled in the art is can.
  • the particle size of the mixture obtained after sieving has different specifications, preferably 3350 ⁇ 106 ⁇ , more preferably 850 ⁇ 425 ⁇ , 600 ⁇ 300 ⁇ , 425 ⁇ 250 ⁇ , 425 ⁇ 212 ⁇ or 212 ⁇ 106 ⁇ .
  • the mixture is fired and divided to obtain a petroleum chopping pressure proppant for fly ash.
  • the burning place of the present invention is not particularly limited, and is preferably 1100 to 1300 ° C, more preferably 1220 to 1280 ° C in a rotary kiln, and the firing time is preferably 4 to 8 h, It is preferably 5 to 7 hours.
  • the invention prepares a petroleum fracturing proppant made of fly ash by using fly ash, potassium feldspar powder and bauxite powder as raw materials.
  • the invention uses low-cost fly ash as a main raw material, in the preparation process, raw materials the ⁇ 1 2 0 3 mullite, surplus feed is converted to Si0 2 as the secret low phosphorus minerals such as quartz, to reduce the apparent density of the product.
  • K 2 0 in potassium feldspar powder as a mineralizer, a liquid phase which accounts for 30% to 40% of the total volume of the raw materials is formed in the raw materials mixed at a high temperature, and the liquid phase formed not only has a large surface tension, but also has a good wetting property.
  • the material is denser and therefore increases the strength of the petroleum fracturing proppant. Moreover, when ⁇ 1 2 0 3 and SiO 2 in the raw material are dissolved to a certain concentration, they react with each other to form acicular mullite crystallization, and then continuously dissolve and crystallization, so that the mullite is changed from a solid phase reaction to a liquid phase reaction. This greatly speeds up the reaction and reduces the temperature required for the reaction. At the same time as the mullite liquefaction, due to the action of the mineralizer, the surplus Si0 2 is converted into a double-headed pseudo-phosphorus quartz crystal, so that the finished product has higher strength.
  • the invention adopts a composite mineralizer formed by potassium feldspar powder and manganese ore powder as a mineralizer for preparing a petroleum fracturing proppant, and the preparation method is as follows:
  • a petroleum cracking proppant made of fly ash is obtained.
  • the invention firstly mixes the fly ash, the manganese ore powder, the potassium feldspar powder and the bauxite powder, and performs the homogenization and refinement treatment, and the manner of the homogenization refining treatment is not particularly limited, and the specific method is:
  • the fly ash, manganese ore powder, potassium feldspar powder and bauxite powder are placed in a forced mixer for homogenization and refining treatment.
  • the invention carries out the homogenization and refinement treatment of the raw materials, so that the particle size distribution of the raw materials is more uniform, the chemical reaction is more smooth, and the chemical reaction is carried out more fully, so that the grain of the petroleum fracturing proppant is finer and the oil fracturing is improved.
  • the strength of the proppant is used to be used.
  • the fly ash, manganese ore powder, potassium feldspar powder and bauxite powder are placed in a forced mixer for homogenization and refining treatment, and after granulation, they are sieved to obtain a mixture.
  • the granulation method of the present invention is not particularly limited, and the granulation method well known to those skilled in the art may be used; the manner of sieving in the present invention is not particularly limited, and the sieving method well known to those skilled in the art is can.
  • the particle size of the mixture obtained after sieving has different specifications, and is preferably 3350 to 106 ⁇ m, more preferably 850 to 425 ⁇ m, 600 to 300 ⁇ m, 425 to 250 ⁇ m, 425 to 212 ⁇ m or 212 to 106 ⁇ m.
  • the mixture is fired and divided to obtain a petroleum chopping pressure proppant for fly ash.
  • the burning place of the present invention is not particularly limited, and is preferably 1100 to 1150 ° C, more preferably 1110 to 1130 ° C in a rotary kiln, and the firing time is preferably 4 to 8 h, It is preferably 5 to 7 hours.
  • the invention prepares a fly ash petroleum fracturing proppant by using fly ash, potassium feldspar powder, manganese ore powder and bauxite powder as raw materials, and the invention uses low-cost fly ash as raw material in the preparation process. ⁇ 1 2 0 3 in the raw material generates mullite, and the surplus SiO 2 in the raw material is converted into a low-viscosity mineral such as phosphorus quartz, which reduces the apparent density of the product.
  • a liquid phase containing 30% to 40% of the total volume of the raw materials is formed in the raw materials mixed at a high temperature, and the liquid phase formed is not only the liquid phase but also the liquid phase formed.
  • the surface tension is large, the wetting performance is good, and the material is denser, thus increasing the strength of the petroleum fracturing proppant.
  • the liquid phase has a strong dissolving ability for A1 2 0 3 and SiO 2 in the raw material at 1100 ° C, and when the A1 2 0 3 and SiO 2 in the raw material are dissolved to a certain concentration, they react with each other to form a needle shape.
  • the mullite is crystallized and then continuously dissolved and crystallized to change the mullite from a solid phase reaction to a liquid phase reaction, which greatly accelerates the reaction rate and The temperature required for the reaction is lowered.
  • the surplus Si0 2 is converted into a double-headed pseudo-phosphorus quartz crystal, so that the finished product has higher strength.
  • 70% of the bauxite powder is mixed and subjected to homogenization and refining processing by a forced mixer, and then granulated, and a mixture having a particle diameter of 900 to 600 ⁇ m is obtained by sieving, and the mixture is used at a pressure of 2.5 m x 45 m under normal pressure.
  • the rotary kiln of the specification is fired at 1180 ° C ⁇ 1220 ° C for 4 hours, and after cooling and sieving, a fly ash petroleum fracturing proppant with a mesh number of 20-40 mesh (850 ⁇ 425 ⁇ ) can be obtained.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.60 g/cm 3 and an apparent density of 2.7 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15 Kg potassium feldspar powder, 25 Kg aluminum content 70% aluminum bauxite powder were mixed and homogenized and refined by a forced mixer, and then granulated and sieved to obtain granules.
  • a mixture having a diameter of 900 to 600 ⁇ m and the mixture is fired at a pressure of 1140 ° C to 1200 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln. After cooling and sieving, the mesh number is 20 ⁇ 40 mesh (850 ⁇ 425 ⁇ ) of fly ash petroleum fracturing proppant.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.56 g/cm 3 and an apparent density of 2.66 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15Kg potassium feldspar powder, 5Kg manganese ore powder, 20Kg aluminum content 70% aluminum bauxite powder are mixed and homogenized and refined by forced mixer, and then granulated, sieved A mixture having a particle diameter of 900 to 600 ⁇ m is obtained, and the mixture is fired at a temperature of 1120 ° C to 1150 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln, and the mesh is obtained after cooling and sieving. It is a petroleum fracturing proppant for fly ash of 20 ⁇ 40 mesh (850 ⁇ 425 ⁇ ).
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.50 g/cm 3 and an apparent density of 2.55 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.55 g/cm 3 and an apparent density of 2.66 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • 30Kg of bauxite powder with 70% aluminum content is mixed and subjected to homogenization and refining processing by a forced mixer, and then granulated, and a mixture having a particle diameter of 900 to 600 ⁇ m is obtained by sieving, and the mixture is used under normal pressure with 2.5.
  • the rotary kiln with a size of x45 m is fired at 1120 ° C ⁇ 1150 ° C for 4 hours. After cooling and sieving, a fly ash petroleum fracturing proppant with a mesh size of 20 to 40 mesh (850 ⁇ 425 ⁇ ) can be obtained. .
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.53 g/cm 3 and an apparent density of 2.65 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.60 g/cm 3 and an apparent density of 2.7 g/cm 3 , and the breaking rate was ⁇ 5% at a closing pressure of 86 MPa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15 Kg potassium feldspar powder, 25 Kg aluminum content 70% aluminum bauxite powder were mixed and homogenized and refined by a forced mixer, and then granulated and sieved to obtain granules.
  • a mixture having a diameter of 710 to 425 ⁇ m and the mixture is fired at a pressure of 1140 ° C to 1200 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln. After cooling and sieving, the mesh number is 30. ⁇ 50 mesh (600 ⁇ 300 ⁇ ) of fly ash petroleum fracturing proppant.
  • the fly ash-made petroleum fracturing proppant was measured to have a bulk density of 1.57 g/cm 3 and an apparent density of 2.67 g/cm 3 , and the breaking rate was ⁇ 5% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.56 g/cm 3 and an apparent density of 2.66 g/cm 3 , and the breaking rate was ⁇ 5% at a closing pressure of 86 MPa.
  • bauxite powder with 70% aluminum content 20Kg is mixed and subjected to homogenization and refining processing by a forced mixer. After granulation, a mixture having a particle diameter of 710 to 425 ⁇ m is obtained by sieving, and the mixture is fired at a temperature of 1120 ° C to 1150 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln. After the separation, a fly ash petroleum fracturing proppant with a mesh size of 30 to 50 mesh (600 ⁇ 300 ⁇ ) can be obtained.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.52 g/cm 3 and an apparent density of 2.58 g/cm 3 , and the breaking rate was ⁇ 6% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.53 g/cm 3 and an apparent density of 2.66 g/cm 3 , and the breaking rate was ⁇ 5% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.51 g/cm 3 and an apparent density of 2.65 g/cm 3 , and the breaking rate was ⁇ 6% at a closing pressure of 86 MPa.
  • the volume density of the petroleum fracturing proppant made of the fly ash is determined to be 1.60 g/cm 3 , apparent density It is 2.7 g/cm 3 , and the breaking rate is ⁇ 8% at a closing pressure of 86 Mpa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15 Kg potassium feldspar powder, 25 Kg aluminum content 70% aluminum bauxite powder were mixed and homogenized and refined by a forced mixer, and then granulated and sieved to obtain granules.
  • a mixture having a diameter of 500 to 425 ⁇ m and the mixture is fired at a pressure of 1140 ° C to 1200 ° C for 4 hours under a normal pressure in a 2.5 m x 45 m rotary kiln. After cooling and sieving, the mesh number is 40. ⁇ 60 mesh (425 ⁇ 250 ⁇ ) of fly ash petroleum fracturing proppant.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.57 g/cm 3 and an apparent density of 2.68 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.56 g/cm 3 and an apparent density of 2.67 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15Kg potassium feldspar powder, 5Kg manganese ore powder, 20Kg aluminum content 70% aluminum bauxite powder are mixed and homogenized and refined by forced mixer, and then granulated, sieved A mixture having a particle diameter of 500 to 425 ⁇ m is obtained, and the mixture is fired at a temperature of 1120 ° C to 1150 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln, and the mesh is obtained after cooling and sieving. It is a 40-60 mesh (425 ⁇ 250 ⁇ ) fly ash petroleum fracturing proppant.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.53 g/cm 3 and an apparent density of 2.60 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.54 g/cm 3 and an apparent density of 2.67 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.53 g/cm 3 and an apparent density of 2.66 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.60 g/cm 3 and an apparent density of 2.7 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15 Kg potassium feldspar powder, 25 Kg aluminum content 70% aluminum bauxite powder were mixed and homogenized and refined by a forced mixer, and then granulated and sieved to obtain granules.
  • a mixture having a diameter of 500 to 355 ⁇ m and the mixture is fired at a pressure of 1140 ° C to 1200 ° C for 4 hours under a normal pressure in a rotary kiln of 2.5 m x 45 m. After cooling and sieving, the mesh number is 40. ⁇ 70 mesh (425 ⁇ 212 ⁇ ) of fly ash petroleum fracturing proppant.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.57 g/cm 3 and an apparent density of 2.68 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.
  • 70% of the bauxite powder is mixed and subjected to homogenization and refining processing by a forced mixer, and then granulated, and a mixture having a particle diameter of 500 to 355 ⁇ m is obtained by sieving, and the mixture is used at a pressure of 2.5 m x 45 m under normal pressure.
  • the rotary kiln of the specification is fired at 1140 ° C ⁇ 1220 ° C for 4 hours, and after cooling and sieving, a fly ash petroleum fracturing proppant with a mesh number of 40 to 70 mesh (425 ⁇ 212 ⁇ ) can be obtained.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.56 g/cm 3 and an apparent density of 2.67 g/cm 3 , and the breaking rate was ⁇ 8% at a closing pressure of 86 MPa.
  • 60Kg Hebi Wanhe Power Plant dust removal waste ash, 15Kg potassium feldspar powder, 5Kg manganese ore powder, 20Kg aluminum content 70% aluminum bauxite powder are mixed and homogenized and refined by forced mixer, and then granulated, sieved A mixture having a particle diameter of 500 to 355 ⁇ m is obtained, and the mixture is fired at a temperature of 1120 ° C to 1150 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln, and the mesh is obtained after cooling and sieving. It is a 40-70 mesh (425 ⁇ 212 ⁇ ) fly ash petroleum fracturing proppant.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.54 g/cm 3 and an apparent density of 2.67 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.
  • Example 24 40Kg Hebi Wanhe Power Plant dust removal waste ash, 25Kg potassium feldspar powder, 5Kg manganese ore powder, 30Kg aluminum content 70% aluminum bauxite powder, mixed and homogenized and refined by forced mixer, and then granulated, sieved A mixture having a particle diameter of 500 to 355 ⁇ m is obtained, and the mixture is fired at a temperature of 1120 ° C to 1150 ° C for 4 hours under a normal pressure using a 2.5 m x 45 m rotary kiln, and the mesh is obtained after cooling and sieving. It is a 40-70 mesh (425 ⁇ 212 ⁇ ) fly ash petroleum fracturing proppant.
  • the fly ash petroleum fracturing proppant was measured to have a bulk density of 1.53 g/cm 3 and an apparent density of 2.66 g/cm 3 , and the breaking rate was ⁇ 7% at a closing pressure of 86 MPa.

Abstract

本发明提供了一种粉煤灰制石油压裂支撑剂，由以下组分制备而成： 1wt%~60wt%的粉煤灰；1wt%~30wt%的钾长石粉；余量为铝矾土粉。本发明以成本低的粉煤灰为原料，在制备过程中，粉煤灰中的Al2O3生成莫来石，原料中富余的SiO2转化为磷石英等低视密矿物，降低了产品的视密度。利用钾长石粉中的K2O作为矿化剂，使物料更致密，因此，增大了石油压裂支撑剂的强度。而且当原料中的Al2O3和SiO2溶解到一定浓度时，相互反应生成针状莫来石析晶而出，然后不断溶解和析晶，使莫来石化从固相反应变为液相反应，这就大大加快了反应速度和降低了反应所需的温度。

Description

一种粉煤灰制石油压裂支撑剂及其制备方法
本申请要求于 2013 年 04 月 25 日提交中国专利局、 申请号为 201310148261.3、 发明名称为 "一种粉煤灰制石油压裂支撑剂及其制备方 法" 的中国专利申请的优先权， 其全部内容通过引用结合在本申请中。 技术领域
本发明属于石油压裂支撑剂技术领域，具体涉及一种粉煤灰制石油压 裂支撑剂及其制备方法。 背景技术
在油田油气开采中， 为提高油井产量， 延长油井高产寿命， 开采难动 用资源而广泛采用压裂工艺。 为防止地下压裂缝的闭合， 保留油气通道， 保持导流能力， 必须使用支撑剂填充裂缝。 由于油层深度不同， 油质黏度 不同， 对支撑剂的性能如强度， 视密度， 粒度大小要求也不相同。 压裂支 撑剂按照体积密度分为高密高强， 中密高强和低密高强三大类，近年来又 出现了对支撑剂超低密度的需求。 目前市场上压裂支撑剂的常用粒度有 16~30目（ 1180~600μηι )、 20~40目（850~425μηι)、 30~50目（600~300μηι )、 40-60目 （ 425~250μηι ) 目和 40~70目 （ 425~212μηι )等多种规格， 但是， 无论何种品种和规格， 石油压裂支撑剂要在具有足够的抗破碎能力前提 下， 具有较低的视密度， 以利于降低压裂成本， 保证对压裂缝填充的饱和 度， 提高油井产量。
目前石油压裂支撑剂生产普遍以高铝矾土为主要原料，辅以一种或几 种金属氧化物做矿化剂，如氧化锰、氧化钙、氧化铁、氧化镁、锆英石等。 申请号为 02112746.8的中国专利公开的压裂支撑剂， 主要原料为 45wt%~55wt。/ 々熟铝矾土、 10wt%~30wt%的高岭土和 20wt%~35wt。/c^宜 兴产红泥。 将上述原料粉碎、 混料、 成球、 烧结， 得到压裂支撑剂。 申请 号为 93111983.9的中国专利公开的压裂支撑剂，主料为 70%~90%的熟铝矾 土经焙烧和粉碎后 ,再加入多组分氧化物与软质粘土组成的辅料共磨和加 水或有机溶剂混碾， 然后经松解、 成球、 筛分、 烧结、 抛光和再次筛分， 得到压裂支撑剂。 申请号为 02157202.X的中国专利公开的压裂支撑剂，其 制备方法为： 90%~94%的高品位生铝矾土，外加 6%~10%的氧化锰矿石粉， 经 1330°C~1350°C高温烧成。 申请号为 02157202.X的中国专利是目前支撑 剂生产创业普遍采用的配方，但是该专利提供的压裂支撑剂依靠特级铝矾 土或一级铝矾土和 Mn02, 含量在 50%以上的锰矿石等优质资源在较高的 温度下制备而成， 因此， 制备过程中高能耗， 高资源消耗限制了压裂支撑 剂的进一步的发展。 发明内容
有鉴于此，本发明要解决的技术问题在于提供一种粉煤灰制石油压裂 支撑剂及其制备方法，本发明采用低成本的粉煤灰为原料，在较低的温度 下制备得到的石油压裂支撑剂视密度小、抗破碎能力强， 并且成本低， 减 少了能源消耗。
本发明提供了一种粉煤灰制石油压裂支撑剂， 由以下组分制备而成： lwt%~60wt%的粉煤灰；
lwt%~30wt%的钾长石粉；
余量为铝矾土粉。
优选的， 所述石油压裂支撑剂还包括 0wt%~5wt%的锰矿粉。
优选的， 所述锰矿粉中 Mn02 占所述粉煤灰制石油压裂支撑剂的 0wt%~5wt%。
优选的， 所述铝矾土粉的铝含量为 35wt%~75wt%。
优选的， 所述石油压裂支撑剂的体积密度≤1.60g/cm3 , 视密度 ≤2.70g/cm3。
本发明还提供了一种粉煤灰制石油压裂支撑剂的制备方法，包括以下 步骤：
A )将粉煤灰、 钾长石粉和铝矾土粉混合， 进行均化细化处理， 经过 制粒后筛分， 得到混合物；
B )将所述混合物烧制、 筛分后， 得到粉煤灰制石油裂压支撑剂。 优选的， 所述制备方法为： a )将粉煤灰、 锰矿粉、 钾长石粉和铝矾土粉混合， 进行均化细化处 理， 经过制粒后筛分， 得到混合物；
b )将所述混合物烧制、 筛分后， 得到粉煤灰制石油裂压支撑剂。 优选的， 所述混合物的粒径为 3350~106μηι。
优选的， 所述步骤 a )具体为：
将粉煤灰， 钾长石粉、锰矿粉和铝矾土粉混合， 置于强制混合机中进 行均化细化处理后， 经过制粒后筛分， 得到混合物。
优选的， 所述烧制的时间为 4~8h。
与现有技术相比，本发明以粉煤灰、钾长石粉和铝矾土粉为原料制备 了一种粉煤灰制石油压裂支撑剂，本发明以成本低的粉煤灰为原料，在制 备过程中， 粉煤灰中的 A1203生成莫来石， 原料中富余的 Si02转化为磷 石英等低视密矿物， 降低了产品的视密度。 利用钾长石粉中的 K20作为 矿化剂， 使在高温下混合的原料中形成占原料总体积 30%~40%的液相， 生成的液相不但表面张力大， 浸润性能好， 使物料更致密， 因此， 增大了 石油压裂支撑剂的强度。 而且当原料中的 Α1203和 Si02溶解到一定浓度 时，相互反应生成针状莫来石析晶而出， 然后不断溶解和析晶， 使莫来石 化从固相反应变为液相反应，这就大大加快了反应速度和降低了反应所需 的温度。 在莫来石液化的同时， 由于矿化剂的作用， 富余的 Si02转变为 双头予状磷石英晶体， 使成品具有较高的强度。
结果表明， 本发明所提供的粉煤灰制石油裂压支撑剂的体积密度
<1.60g/cm3, 视密度≤2.70g/cm3, 在 86MPa的闭合压力下， 破碎率≤8%。 具体实施方式
本发明提供了一种粉煤灰制石油压裂支撑剂， 由以下组分制备而成： lwt%~60wt%的粉煤灰；
lwt%~30wt%的钾长石粉；
余量为铝矾土粉。
本发明以粉煤灰作为石油压裂支撑剂的主要原料,粉煤灰为工业废弃 物， 成本低， 因此， 将粉煤灰合理利用具有节能环保、 节约资源的重要意 义。 其中， 粉煤灰占原料总量的质量范围优选为 lwt%~60wt%, 更优选为 30wt%~55wt%, 最优选为 40wt%~50wt%。
所述钾长石粉为石油压裂支撑剂的矿化剂，其中，钾长石粉中的 K20 起到矿化作用。 所述钾长石粉的添加量占原料总量的质量范围优选为 lwt%~30wt%, 更优选为 10wt%~25wt%, 最优选为 15wt%~20wt%。
在本发明中， 采用铝矾土粉调节混合后原料中 A1203、 Si02的含量， 所述铝矾土粉中铝含量为 35wt%~75wt%, 更优选为 50wt%~70wt%。所述 铝矾土优选采用三级铝矾土或熟铝矾土，更优选为三级铝矾土。在确定粉 煤灰和钾长石粉的添加量后，所添加的铝矾土粉占原料总量的质量百分数 与粉煤灰、 钾长石粉的质量百分数之和为 100%。
本发明所制备的石油压裂支撑剂的原料中还包括锰矿粉，所述锰矿粉 为辅助矿化剂和染色剂，锰矿粉中的 Mn02占所述粉煤灰制石油压裂支撑 剂的 0wt%~5wt%。 所述锰矿粉的添加量占原料总量的质量范围优选为 0wt%~5wt%, 更优选为 lwt%~4wt%, 最优选为 2wt%~3wt%。
本发明以钾长石粉中的 K20和锰矿粉中的 Mn02形成的复合矿化剂， 使在高温下混合的原料中形成占原料总体积 30%~40%的液相， 生成的液 相不但表面张力大， 浸润性能好， 使物料更致密， 因此， 增大了石油压裂 支撑剂的强度。
本发明所提供的石油压裂支撑剂的体积密度≤1.60g/cm3 , 视密度 ≤2.70g/cm3。 优选的， 所述体积密度≤1.58g/cm3, 视密度≤2.60g/cm3。
本发明还提供了一种粉煤灰制石油压裂支撑剂的制备方法，包括以下 步骤：
A )将粉煤灰、 钾长石粉和铝矾土粉混合， 进行均化细化处理， 经过 制粒后筛分， 得到混合物；
B )将所述混合物烧制、 筛分后， 得到粉煤灰制石油裂压支撑剂。 本发明首先将粉煤灰、钾长石粉和铝矾土粉混合，进行均化细化处理， 对所述均化细化处理的方式并无特殊限制， 具体方法为：
将粉煤灰， 钾长石粉和铝矾土粉置于强制混合机中进行均化细化处 理。 本发明将原料进行均化细化处理， 使原料粒度分布更加均匀， 化学反 应更加顺利，并且化学反应进行的更加充分，使得到的石油压裂支撑剂的 晶粒更细小， 提高了石油压裂支撑剂的强度。 将粉煤灰，钾长石粉和铝矾土粉置于强制混合机中进行均化细化处理 后， 经过制粒后筛分，得到混合物。 本发明对所述制粒的方式并无特殊限 制，本领域技术人员熟知的制粒方式即可；本发明对所述筛分的方式并无 特殊限制， 本领域技术人员熟知的筛分方式即可。 其中， 筛分后得到的混 合物的粒径有不同的规格， 优选为 3350~106μηι, 更优选为 850~425μηι、 600~300μηι、 425~250μηι、 425~212μηι或 212~106μηι。
本发明将所述混合物进行烧制、 分后， 即可得到粉煤灰制石油裂压 支撑剂。本发明对所述烧制的场所并无特殊限制，优选在回转窑中进行烧 为 1100~1300°C , 更优选为 1220~1280°C , 所述烧制的时间优选为 4~8h, 更优选为 5~7h。
烧制、 筛分后得到粉煤灰制石油压裂支撑剂，所述粉煤灰制石油压裂 支撑剂中化学成分重量比例达到： A1203: 40%~48%, Si02:38%~45%, K20: 2%~4%。
本发明以粉煤灰、钾长石粉和铝矾土粉为原料制备了一种粉煤灰制石 油压裂支撑剂， 本发明以成本低的粉煤灰为主要原料， 在制备过程中，原 料中的 Α1203生成莫来石， 原料中富余的 Si02转化为磷石英等低视密矿 物， 降低了产品的视密度。 利用钾长石粉中的 K20作为矿化剂， 使在高 温下混合的原料中形成占原料总体积 30%~40%的液相， 生成的液相不但 表面张力大， 浸润性能好， 使物料更致密， 因此， 增大了石油压裂支撑剂 的强度。 而且当原料中的 Α1203和 Si02溶解到一定浓度时， 相互反应生 成针状莫来石析晶而出，然后不断溶解和析晶，使莫来石化从固相反应变 为液相反应，这就大大加快了反应速度和降低了反应所需的温度。在莫来 石液化的同时， 由于矿化剂的作用， 富余的 Si02转变为双头予状磷石英 晶体， 使成品具有较高的强度。
本发明采用钾长石粉和锰矿粉形成的复合矿化剂作为制备石油压裂 支撑剂的矿化剂， 制备方法为：
a )将粉煤灰、 锰矿粉、 钾长石粉和铝矾土粉混合， 进行均化细化处 理， 经过制粒后筛分， 得到混合物；
b )将所述混合物烧制、 筛分后， 得到粉煤灰制石油裂压支撑剂。 本发明首先将粉煤灰、锰矿粉、钾长石粉和铝矾土粉混合， 进行均化 细化处理， 对所述均化细化处理的方式并无特殊限制， 具体方法为：
将粉煤灰，锰矿粉、钾长石粉和铝矾土粉置于强制混合机中进行均化 细化处理。 本发明将原料进行均化细化处理， 使原料粒度分布更加均匀， 化学反应更加顺利，并且化学反应进行的更加充分，使得到的石油压裂支 撑剂的晶粒更细小， 提高了石油压裂支撑剂的强度。
将粉煤灰，锰矿粉、钾长石粉和铝矾土粉置于强制混合机中进行均化 细化处理后， 经过制粒后筛分， 得到混合物。 本发明对所述制粒的方式并 无特殊限制，本领域技术人员熟知的制粒方式即可；本发明对所述筛分的 方式并无特殊限制， 本领域技术人员熟知的筛分方式即可。 其中， 筛分后 得到的混合物的粒径有不同的规格， 优选为 3350~106μηι, 更优选为 850~425μηι、 600~300μηι、 425~250μηι、 425~212μηι或 212~106μηι。
本发明将所述混合物进行烧制、 分后， 即可得到粉煤灰制石油裂压 支撑剂。本发明对所述烧制的场所并无特殊限制，优选在回转窑中进行烧 为 1100~1150°C , 更优选为 1110~1130°C , 所述烧制的时间优选为 4~8h, 更优选为 5~7h。
烧制结束后得到粉煤灰制石油压裂支撑剂，所述粉煤灰制石油压裂支 撑剂中化学成分重量比例达到： A1203: 40%~48%, Si02:38%~45%, K20: 2%~4%。
本发明以粉煤灰、钾长石粉、锰矿粉和铝矾土粉为原料制备了一种粉 煤灰制石油压裂支撑剂，本发明以成本低的粉煤灰为原料,在制备过程中， 原料中的 Α1203生成莫来石， 原料中富余的 Si02转化为磷石英等低视密 矿物， 降低了产品的视密度。利用钾长石粉中的 K20和锰矿粉中的 Mn02 形成的复合矿化剂， 使在高温下混合的原料中形成占原料总体积 30%~40%的液相， 生成的液相不但表面张力大， 浸润性能好， 使物料更 致密， 因此， 增大了石油压裂支撑剂的强度。 而且该液相在 1100°C对原 料中的 A1203和 Si02就具有了很强的溶解能力，当原料中的 A1203和 Si02 溶解到一定浓度时，相互反应生成针状莫来石析晶而出，然后不断溶解和 析晶，使莫来石化从固相反应变为液相反应，这就大大加快了反应速度和 降低了反应所需的温度。在莫来石液化的同时， 由于矿化剂的作用， 富余 的 Si02转变为双头予状磷石英晶体， 使成品具有较高的强度。
结果表明，本发明所提供的粉煤灰制石油裂压支撑剂的体积密度小于 等于 1.60 g/cm3 ,视密度≤2.70g/cm3 ,在 86MPa的闭合压力下，破碎率≤8%。
为了进一步理解本发明，下面结合实施例对本发明提供的粉煤灰制石 油压裂支撑剂及其制备方法进行说明，本发明的保护范围不受以下实施例 的限制。 实施例 1
将 50Kg鹤壁万和电厂的除尘废灰， 25 Kg钾长石粉， 25 Kg铝含量
70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 900~600μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1180°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 20~40目（850~425μηι)的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.60g/cm3, 视密度 为 2.7 g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例
将 60Kg鹤壁万和电厂的除尘废灰， 15 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 900~600μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1200°C烧制 4个小时，冷却筛分后即可得到目 数为 20~40目（850~425μηι)的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.56g/cm3, 视密度 为 2.66g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 3
将 30Kg鹤壁万和电厂的除尘废灰， 30 Kg钾长石粉， 45 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 900~600μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 20~40目（850~425μηι)的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.56g/cm3, 视密度 为 2.63g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 4
将 60Kg鹤壁万和电厂的除尘废灰， 15Kg钾长石粉， 5Kg锰矿粉， 20Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 900~600μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 20~40目（850~425μηι)的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.50g/cm3, 视密度 为 2.55g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 5
将 30Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉， 40Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 900~600μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1100°C~1120°C烧制 4个小时， 冷却筛 分后即可得到目数为 20~40目（850~425μηι)的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.55g/cm3, 视密度 为 2.66g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 6
将 40Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉，
30Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 900~600μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 20~40目（850~425μηι)的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.53g/cm3, 视密度 为 2.65g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 7
将 50Kg鹤壁万和电厂的除尘废灰， 25 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 710~425μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1180°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 30~50目 （600~300μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.60g/cm3, 视密度 为 2.7 g/cm3, 在 86Mpa闭合压力下， 破碎率≤5%。 实施例 8
将 60Kg鹤壁万和电厂的除尘废灰， 15 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 710~425μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1200°C烧制 4个小时，冷却筛分后即可得到目 数为 30~50目 （600~300μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.57g/cm3, 视密度 为 2.67g/cm3, 在 86Mpa闭合压力下， 破碎率≤5%。 实施例 9
将 30Kg鹤壁万和电厂的除尘废灰， 30 Kg钾长石粉， 45 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 710~425μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 30~50目 （600~300μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.56g/cm3, 视密度 为 2.66g/cm3, 在 86Mpa闭合压力下， 破碎率≤5%。 实施例 10
将 60Kg鹤壁万和电厂的除尘废灰， 15Kg钾长石粉， 5Kg锰矿粉，
20Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 710~425μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 30~50目（ 600~300μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.52g/cm3, 视密度 为 2.58g/cm3, 在 86Mpa闭合压力下， 破碎率≤6%。 实施例 11
将 30Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉， 40Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 710~425μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1100°C~1120°C烧制 4个小时， 冷却筛 分后即可得到目数为 30~50目（ 600~300μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.53g/cm3, 视密度 为 2.66g/cm3, 在 86Mpa闭合压力下， 破碎率≤5%。 实施例 12
将 40Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉， 30Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 710~425μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 30~50目（ 600~300μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.51g/cm3, 视密度 为 2.65g/cm3, 在 86Mpa闭合压力下， 破碎率≤6%。 实施例 13
将 50Kg鹤壁万和电厂的除尘废灰， 25 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 500~425μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1180°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 40~60目 （425~250μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.60g/cm3, 视密度 为 2.7 g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 14
将 60Kg鹤壁万和电厂的除尘废灰， 15 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 500~425μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1200°C烧制 4个小时，冷却筛分后即可得到目 数为 40~60目 （425~250μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.57g/cm3, 视密度 为 2.68g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 15
将 30Kg鹤壁万和电厂的除尘废灰， 30 Kg钾长石粉， 45 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 500~425μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 40~60目 （425~250μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.56g/cm3, 视密度 为 2.67g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 16
将 60Kg鹤壁万和电厂的除尘废灰， 15Kg钾长石粉， 5Kg锰矿粉， 20Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 500~425μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 40~60目（ 425~250μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.53g/cm3, 视密度 为 2.60g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 17
将 30Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉, 40Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 500~425μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1100°C~1120°C烧制 4个小时， 冷却筛 分后即可得到目数为 40~60目（ 425~250μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.54g/cm3, 视密度 为 2.67g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 18
将 40Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉， 30Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 500~425μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 40~60目（ 425~250μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.53g/cm3, 视密度 为 2.66g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 19
将 50Kg鹤壁万和电厂的除尘废灰， 25 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 500~355μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1180°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 40~70目 （425~212μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.60g/cm3, 视密度 为 2.7 g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 20
将 60Kg鹤壁万和电厂的除尘废灰， 15 Kg钾长石粉， 25 Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 500~355μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1200°C烧制 4个小时，冷却筛分后即可得到目 数为 40~70目 （425~212μηι ) 的粉煤灰制石油压裂支撑剂。 测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.57g/cm3, 视密度 为 2.68g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 21
将 30Kg鹤壁万和电厂的除尘废灰， 30 Kg钾长石粉， 45 Kg铝含量
70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而后制粒， 经筛 分取得粒径为 500~355μηι的混合物， 将所述混合物在常压下用 2.5米 x45 米规格的回转窑经 1140°C~1220°C烧制 4个小时，冷却筛分后即可得到目 数为 40~70目 （425~212μηι ) 的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.56g/cm3, 视密度 为 2.67g/cm3, 在 86Mpa闭合压力下， 破碎率≤8%。 实施例 22
将 60Kg鹤壁万和电厂的除尘废灰， 15Kg钾长石粉， 5Kg锰矿粉， 20Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 500~355μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 40~70目（ 425~212μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.54g/cm3, 视密度 为 2.63g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 23
将 30Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉， 40Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 500~355μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1100°C~1120°C烧制 4个小时， 冷却筛 分后即可得到目数为 40~70目（ 425~212μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.54g/cm3, 视密度 为 2.67g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。 实施例 24 将 40Kg鹤壁万和电厂的除尘废灰， 25Kg钾长石粉， 5Kg锰矿粉， 30Kg铝含量 70%的铝矾土粉混合后经强制混合机进行均化细化加工， 而 后制粒， 经筛分取得粒径为 500~355μηι的混合物， 将所述混合物在常压 下用 2.5米 x45米规格的回转窑经 1120°C~1150°C烧制 4个小时， 冷却筛 分后即可得到目数为 40~70目（ 425~212μηι )的粉煤灰制石油压裂支撑剂。
测定所述粉煤灰制石油压裂支撑剂的体积密度为 1.53g/cm3, 视密度 为 2.66g/cm3, 在 86Mpa闭合压力下， 破碎率≤7%。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的 普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进 和润饰， 这些改进和润饰也应视为本发明的保护范围。

Claims

权 利 要 求
1、 一种粉煤灰制石油压裂支撑剂， 由以下组分制备而成：
lwt%~60wt%的粉煤灰；
lwt%~30wt%的钾长石粉；
余量为铝矾土粉。
2、 根据权利要求 1所述的石油压裂支撑剂， 其特征在于， 所述石油 压裂支撑剂还包括 0wt%~5 wt%的锰矿粉。
3、 根据权利要求 2所述的石油压裂支撑剂， 其特征在于， 所述锰矿 粉中 Mn02占所述粉煤灰制石油压裂支撑剂的 0wt%~5wt%。
4、 根据权利要求 1所述的石油压裂支撑剂， 其特征在于， 所述铝矾 土粉的铝含量为 35wt%~75wt%。
5、 根据权利要求 1所述的石油压裂支撑剂， 其特征在于， 所述石油 压裂支撑剂的体积密度≤1.60g/cm3, 视密度≤2.70g/cm3。
6、 一种粉煤灰制石油压裂支撑剂的制备方法， 包括以下步骤：
A )将粉煤灰、 钾长石粉和铝矾土粉混合， 进行均化细化处理， 经过 制粒后筛分， 得到混合物；
B )将所述混合物烧制、 筛分后， 得到粉煤灰制石油裂压支撑剂。
7、根据权利要求 6所述的制备方法， 其特征在于， 所述制备方法为： a )将粉煤灰、 锰矿粉、 钾长石粉和铝矾土粉混合， 进行均化细化处 理， 经过制粒后筛分， 得到混合物；
b )将所述混合物烧制、 筛分后， 得到粉煤灰制石油裂压支撑剂。
8、 根据权利要求 6或 7所述的制备方法， 其特征在于， 所述混合物 的粒径为 3350~106μηι。
9、 根据权利要求 7所述的制备方法， 其特征在于， 所述步骤 a )具 体为：
将粉煤灰， 钾长石粉、锰矿粉和铝矾土粉混合， 置于强制混合机中进 行均化细化处理， 经过制粒后筛分， 得到混合物。
10、根据权利要求 7所述的制备方法， 其特征在于， 所述烧制的时间 为 4~8h。
+
PCT/CN2013/076385 2013-04-25 2013-05-29 一种粉煤灰制石油压裂支撑剂及其制备方法 WO2014172955A1 (zh)

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