CN102352239A - Preparation method of lightweight acid resistant ceramsite fracturing propping agent - Google Patents

Preparation method of lightweight acid resistant ceramsite fracturing propping agent Download PDF

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Publication number
CN102352239A
CN102352239A CN2011102368461A CN201110236846A CN102352239A CN 102352239 A CN102352239 A CN 102352239A CN 2011102368461 A CN2011102368461 A CN 2011102368461A CN 201110236846 A CN201110236846 A CN 201110236846A CN 102352239 A CN102352239 A CN 102352239A
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China
Prior art keywords
sintering
temperature
preparation
raw materials
fracturing propping
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Pending
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CN2011102368461A
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Chinese (zh)
Inventor
吴婷婷
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 CN2011102368461A priority Critical patent/CN102352239A/en
Publication of CN102352239A publication Critical patent/CN102352239A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a preparation method of a lightweight acid resistant ceramsite fracturing propping agent. Raw materials contain: by weight, 70-90% of alumina, 0.1-10% of titanium dioxide and 0-30% of a sintering agent, wherein the sum of the mass percentage of the raw materials is 100% and the sintering agent contains one or more compounds selected from barium, calcium, magnesium and boron. The preparation method provided by the invention comprises the following steps of: putting the raw materials into a ball milling device and carrying out ball milling for 12-48 hours; drying the obtained slurry at the temperature of 60-120 DEG C for 3-12 hours; preparing the obtained raw material into a spherical granular green compact by a molding technology; sintering the obtained granular green compact in a Si-Mo furnace at the temperature of 1300-1550 DEG C, keeping warm for 0.5-3 hours, and cooling with the furnace temperature. Tested according to the SY/T5108-2006 recommended method, the acid solubility of the finished product is less than 0.5%, which reaches the standard requirement in the industry (the allowable value of the acid solubility is less than or equal to 5%). The technology provided by the invention is simple and is suitable for industrial production; in addition, the sintering temperature of the prepared product is low, thus substantially reducing high temperature energy consumption and product cost during the high-alumina ceramic production.

Description

The preparation method of lightweight acidproof ceramic fracturing propping agent
Technical field
The present invention relates to a kind of preparation method of lightweight acidproof ceramic fracturing propping agent.
Background technology
Fracturing propping agents are a kind of proprietary materials of oil gas fracturing technique, are used for supporting rock seam, for the circulation of hydrocarbon flow provides the passage of hypertonicity, keep high flow conductivity, thus improve oil and gas production, prolong the oil gas well the length of service, reduce the oil recovery pneumatolytic this.The quality of fracturing propping agents quality is the key that can oil-gas mining succeed, and wherein acid resistance is one of important indicator.The propping agent that is pressed into the rock seam is wanted to bear various erosion medium resistance in the ground environment, in order to avoid the cracked obstruction pressure break passage in back that is corroded stops gas and oil to flow out.At the aspect of performance of fracturing propping agents, all exist same problem-acid resistance poor both at home and abroad, volume density is high.Present domestic most propping agent manufacturer is a main raw material with bauxitic clay or using industrial solid waste, and the fracturing propping agents acid solubility, the volume density that cooperate other inorganic materials to produce are higher, are difficult to satisfy the requirement of oil-gas mining, influence the output of oil-gas field.The quality of U.S. Carbo company fracturing propping agents has been represented international most advanced level, but the acid solubility of its HSP product also can only reach 3.5%, volume density 3.56g/cm 3Therefore, the acid resistance of raising fracturing propping agents is matters of utmost importance that oil, Natural gas extraction industry must solve.
Jeremiah J.Fitzgibbon; Lafayette; La. wait that to have introduced a kind of be the spheroidal particle fracturing propping agents and the preparation method of main raw material with the clay in the patent (patent No. US4427068) of application, finished acid solubleness is between 4.6-7.4%, and volume density is at 2.7-3.27g/cm 3Application number is 200410010272.6, and patent name is the patent of " high-strength ceramic proppant and preparation method thereof ", discloses a kind of ceramsite propping agent and working method thereof, and finished acid solubleness is 4.26%.So far, the propping agent product of acid solubility<0.5% does not appear in the newspapers.
Summary of the invention
The objective of the invention is provides a kind of acidproof ceramic fracturing propping agent and preparation method to the general higher present situation of domestic and international fracturing propping agents acid solubility.Adopt industrial raw material,, prepare the acidproof ceramic fracturing propping agent of acid solubility<0.5% through adding the compound of titanium.
Concrete steps are:
(1) raw materials quality per-cent is: aluminum oxide 70-90%, titanium dioxide 0.1-10%, sintering agent 0-30%; The mass percent sum of raw material is 100%, and sintering agent is one or more in the compound of barium, calcium, magnesium and boron;
(2) step (1) raw material being put into ball mill device carried out ball milling 12-48 hour;
(3) step (2) gained slurry was dried 3-12 hour under 60 ℃ of-120 ℃ of temperature;
(4) with step (3) gained material through moulding process, process the form of spherical particles green compact;
(5) with step (4) gained particulate green 1300 ℃ of-1550 ℃ of sintering in silicon molybdenum stove, be incubated 0.5-3 hour, get final product with the furnace temperature cooling.
According to the SY/T5108-2006 recommend method finished product is tested, acid solubility<0.5% reaches the requirement (permissible value of acid solubility≤5%) of industry standard.
The present invention adopts general industry equipment, and technology is simple, help suitability for industrialized production; The product sintering temperature of preparation is low, can significantly reduce high temperature energy consumption and product cost in the high alumina ceramic production.
Embodiment
Embodiment 1:
(1) prepares burden according to mass percent: α-Al 2O 3Powder 85%, titanium dioxide 1%, barium carbonate 6%, Natural manganese dioxide 8%;
(2) step (1) gained material was put into the ball mill device ball mill mixing 24 hours;
(3) step (2) gained slurry was dried 5 hours under 100 ℃ of temperature;
(4) with step (3) gained material through moulding process, process the form of spherical particles green compact;
(5) with step (4) gained particulate green 1450 ℃ of sintering in silicon molybdenum stove, be incubated 1 hour, cool off with furnace temperature.
The acid solubility of products obtained therefrom is 0.2%, and volume density is 2.2g/cm 3
Embodiment 2:
(1) raw materials quality per-cent is: α-Al 2O 3Powder 86%, titanium dioxide 4%, barium carbonate 3%, Natural manganese dioxide 7%;
(2) step (1) raw material is put into ball mill device and carried out ball milling 24 hours;
(3) step (2) gained slurry was dried 5 hours under 100 ℃ of temperature;
(4) with step (3) gained material through moulding process, process the form of spherical particles green compact;
(5) with step (4) gained particulate green 1400 ℃ of sintering in silicon molybdenum stove, be incubated 1 hour, cool off with furnace temperature.
The acid solubility of products obtained therefrom is 0.15%, and volume density is 3.2g/cm 3
Embodiment 3:
(1) raw materials quality per-cent is: α-Al 2O 3Powder 88%, titanium dioxide 7%, barium carbonate 2%, Natural manganese dioxide 3%;
(2) step (1) raw material is put into ball mill device and carried out ball milling 24 hours;
(3) step (2) gained slurry was dried 5 hours under 100 ℃ of temperature;
(4) with step (3) gained material through moulding process, process the form of spherical particles green compact;
(5) with step (4) gained particulate green 1450 ℃ of sintering in silicon molybdenum stove, be incubated 1 hour, cool off with furnace temperature.
The acid solubility of products obtained therefrom is 0.45%.

Claims (1)

1. the preparation method of a ceramic fracturing propping agent is characterized in that concrete steps are:
(1) raw materials quality per-cent is: aluminum oxide 70-90%, titanium dioxide 0.1-10%, sintering agent 0-30%; The mass percent sum of raw material is 100%, and sintering agent is one or more in the compound of barium, calcium, magnesium and boron;
(2) step (1) raw material being put into ball mill device carried out ball milling 12-48 hour;
(3) step (2) gained slurry was dried 3-12 hour under 60 ℃ of-120 ℃ of temperature;
(4) with step (3) gained material through moulding process, process the form of spherical particles green compact;
(5) with step (4) gained particulate green 1300 ℃ of-1550 ℃ of sintering in silicon molybdenum stove, be incubated 0.5-3 hour, get final product with the furnace temperature cooling.
CN2011102368461A 2011-08-16 2011-08-16 Preparation method of lightweight acid resistant ceramsite fracturing propping agent Pending CN102352239A (en)

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CN2011102368461A CN102352239A (en) 2011-08-16 2011-08-16 Preparation method of lightweight acid resistant ceramsite fracturing propping agent

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Application Number Priority Date Filing Date Title
CN2011102368461A CN102352239A (en) 2011-08-16 2011-08-16 Preparation method of lightweight acid resistant ceramsite fracturing propping agent

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CN102352239A true CN102352239A (en) 2012-02-15

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659393A (en) * 2012-05-27 2012-09-12 桂林理工大学 Preparation method of medium- and low-density fracturing propping agent with fine acid resistance

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101811873A (en) * 2010-04-08 2010-08-25 桂林理工大学 Method for preparing silicon-free or low-silicon acidproof ceramic fracturing propping agent

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101811873A (en) * 2010-04-08 2010-08-25 桂林理工大学 Method for preparing silicon-free or low-silicon acidproof ceramic fracturing propping agent

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《中国陶瓷》 20100215 赵艳荣等 "高铝陶粒支撑剂的研制" 第46-50页 1 第46卷, 第2期 *
赵艳荣等: ""高铝陶粒支撑剂的研制"", 《中国陶瓷》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659393A (en) * 2012-05-27 2012-09-12 桂林理工大学 Preparation method of medium- and low-density fracturing propping agent with fine acid resistance

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Application publication date: 20120215