CN105837183A - Preparation method of ceramsite fracturing propping agent with excellent acid resistance - Google Patents

Preparation method of ceramsite fracturing propping agent with excellent acid resistance Download PDF

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Publication number
CN105837183A
CN105837183A CN201610171156.5A CN201610171156A CN105837183A CN 105837183 A CN105837183 A CN 105837183A CN 201610171156 A CN201610171156 A CN 201610171156A CN 105837183 A CN105837183 A CN 105837183A
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China
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compound
thulium
mass percent
fracturing propping
propping agent
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CN201610171156.5A
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马俊良
吴伯麟
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Guilin University of Technology
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Guilin University of Technology
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Priority to CN201610171156.5A priority Critical patent/CN105837183A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped 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 aluminium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208Calcium oxide or oxide-forming salts thereof, e.g. lime
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/349Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a preparation method of a ceramsite fracturing propping agent with excellent acid resistance. The preparation method comprises the following steps: (1) preparing the following raw materials (by weight): 10-99% of alumina, 0.01-80% of a rare-earth thulium compound and 0.1-15% of a composite additive which is one or more ingredients selected from compounds of calcium, magnesium and silicon or mineral; (2) ball-milling the materials prepared in the Step (1) by a ball mill for 15-50 h; (3) drying slurry obtained in the Step (2) and granulating to prepare a green body; and (4) sintering the green body obtained in the Step (3) at 1300-1700 DEG C, carrying out thermal insulation for 0.5-2 h, and cooling to room temperature. By testing the ceramsite fracturing propping agent according to SY/T5108-2006, acid solubility can be lowered to 0.0147% and is greatly lower than the industrial standard (being less than or equal to 5.0%). The raw materials of the product have wide sources; the production technology is simple; and the prepared ceramsite fracturing propping agent has good acid resistance.

Description

The preparation method of the ceramic fracturing propping agent that a kind of acid resistance is excellent
Technical field
The present invention relates to the preparation method of the excellent ceramic fracturing propping agent of a kind of acid resistance.
Background technology
The exploitation of oil gas pressure break is to safeguard oil gas field volume increase, the important technology of stable yields, for low-permeability and ultra-deep oil-gas reservoir Exploitation particularly important.Fracturing propping agents be oil gas fracturing technique must use material.Proppant is in the underground work as deep as several kms Make, be used for supporting rock seam, for the passage of the circulation offer high osmosis of gas stream.Therefore, they must be able to bear in the earth's crust Pressure and various corrosive medium and the erosion of fracturing fluid.The quality of fracturing propping agents performance has great shadow to the effect of exploitation Ring.Acid solubility is one of important indicator of fracturing propping agents quality good or not.If acid resistance is bad, fracturing propping agents are in corruption Rough coat is there will be during erosion, dry linting, the phenomenon such as even broken, thus block the passage of oil, gas, weaken flow conductivity.
At present, the fracturing propping agents acid resistance of domestic product is the most poor, and general acid solubility is between 8-10%, not The requirement (≤5%) of industry standard can be reached.Carbo company of the U.S. is proppant manufacturer the most maximum, and it produces Quality is in a leading position level in the world.During the said firm is used for, the fracturing propping agents acid solubility of deep oil well be 3.5-4.5%. Although reached the requirement of industry standard, but still higher.Improve acid resistance and have become as a technology of proppant industry A difficult problem.
Summary of the invention
It is an object of the invention to the ceramic fracturing propping agent providing a kind of acid resistance excellent for the problem of above-mentioned existence Preparation method.
Concretely comprise the following steps:
(1) feed components mass percent is: aluminium oxide: 10-99%, the compound 0.01-80% of rare earth thulium, compound additive 0.1-15%, the mass percent sum of raw material is 100%, and compound additive is in the compound of calcium, magnesium and silicon or mineral Plant or multiple.
(2) material that step (1) prepares is put into ball milling 15-50 hour in ball mill device.
(3), after slurry step (2) obtained is dried, green compact are made in pelletize.
(4) by step (3) gained green compact at 1300-1700 DEG C of sintering, it is incubated 0.5-2 hour, is cooled to room temperature, obtains haydite Fracturing propping agents.
(5) by standard: SY/T5108 2006 carries out acid solubility test to ceramic fracturing propping agent.
The compound of described rare earth thulium is in Dithulium trioxide, thulium carbonate, thulium nitrate, thulium oxalate, phosphoric acid thulium and thulium hydroxide A kind of.
The compound of described calcium be calcium oxide mass percent more than 45% compound, the mineral of calcic be limestone, One in aragonite, anorthite, calcite, dolomite and chalk rock.
The compound of described silicon be silicon oxide mass percent more than 35% compound, siliceous mineral be Kaolin, One in diopside, montmorillonite, pyrophillite, Talcum and serpentine.
The compound of described magnesium be magnesium oxide mass percent more than 45% compound, the mineral containing magnesium be shepardite, One in magnesite and dolomite.
Raw material of the present invention is extensive, and production technology is simple, and the acid resistant property of porcelain granule fracturing propping agent prepared is good.
Detailed description of the invention
Embodiment 1:
(1) feed components mass percent is: aluminium oxide: 85%, Kaolin 3.33%, calcite 3.33%, dolomite 3.34% With Dithulium trioxide (Tm2O3) 5%.
(2) material that step (1) prepares is put into ball milling 20 hours in ball mill device.
(3), after slurry step (2) obtained is dried, green compact are made in pelletize.
(4) by step (3) gained green compact at 1365 DEG C of sintering, it is incubated 1 hour, is cooled to room temperature and prepares ceramic fracturing support Agent.
(5) by standard: SY/T5108 2006 carries out acid solubility test to ceramic fracturing propping agent, acid solubility is 0.387%。
Embodiment 2:
(1) feed components mass percent is: aluminium oxide: 10%, Kaolin 3.33%, calcite 3.33%, dolomite 3.34% With Dithulium trioxide (Tm2O3) 80%.
(2) material that step (1) prepares is put into ball milling 30 hours in ball mill device.
(3), after slurry step (2) obtained is dried, green compact are made in pelletize.
(4) by step (3) gained green compact at 1630 DEG C of sintering, it is incubated 1.5 hours, is cooled to room temperature and prepares ceramic fracturing and prop up Support agent.
(5) by standard: SY/T5108 2006 carries out acid solubility test to ceramic fracturing propping agent, acid solubility is 0.0147%。

Claims (1)

1. the preparation method of a ceramic fracturing propping agent, it is characterised in that concretely comprise the following steps:
Feed components mass percent is: aluminium oxide: 10-99%, the compound 0.01-80% of rare earth thulium, compound additive 0.1-15%, the mass percent sum of raw material is 100%, and compound additive is in the compound of calcium, magnesium and silicon or mineral Plant or multiple;
The material that step (1) prepares is put into ball milling 15-50 hour in ball mill device;
After slurry step (2) obtained is dried, green compact are made in pelletize;
By step (3) gained green compact at 1300-1700 DEG C of sintering, it is incubated 0.5-2 hour, is cooled to room temperature, obtain ceramic fracturing and prop up Support agent;
The compound of described rare earth thulium is the one in Dithulium trioxide, thulium carbonate, thulium nitrate, thulium oxalate, phosphoric acid thulium and thulium hydroxide;
The compound of described calcium is the mass percent of the calcium oxide compound more than 45%, and the mineral of calcic are limestone, literary composition One in stone, anorthite, calcite, dolomite and chalk rock;
The compound of described silicon is the mass percent of the silicon oxide compound more than 35%, and siliceous mineral are Kaolin, saturating brightness One in stone, montmorillonite, pyrophillite, Talcum and serpentine;
The compound of described magnesium is the mass percent of the magnesium oxide compound more than 45%, and the mineral containing magnesium are shepardite, magnesite One in ore deposit and dolomite.
CN201610171156.5A 2016-03-24 2016-03-24 Preparation method of ceramsite fracturing propping agent with excellent acid resistance Pending CN105837183A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1180696A (en) * 1967-12-29 1970-02-11 Westinghouse Electric Corp Ceramic to Metal Seals for Containing High Temperature Vapors
CN104987049A (en) * 2015-08-16 2015-10-21 桂林理工大学 Preparation method of acid-resisting alumina based ceramsite fracturing propping agent
CN105236940A (en) * 2015-09-11 2016-01-13 桂林理工大学 Method for preparing acid resistance ceramsite fracturing propping agent by using rare earth compound

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1180696A (en) * 1967-12-29 1970-02-11 Westinghouse Electric Corp Ceramic to Metal Seals for Containing High Temperature Vapors
CN104987049A (en) * 2015-08-16 2015-10-21 桂林理工大学 Preparation method of acid-resisting alumina based ceramsite fracturing propping agent
CN105236940A (en) * 2015-09-11 2016-01-13 桂林理工大学 Method for preparing acid resistance ceramsite fracturing propping agent by using rare earth compound

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Application publication date: 20160810