CN102942368A - Method for preparing high-strength petroleum fracturing propping agent from low-grade bauxite - Google Patents
Method for preparing high-strength petroleum fracturing propping agent from low-grade bauxite Download PDFInfo
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- CN102942368A CN102942368A CN2012104988092A CN201210498809A CN102942368A CN 102942368 A CN102942368 A CN 102942368A CN 2012104988092 A CN2012104988092 A CN 2012104988092A CN 201210498809 A CN201210498809 A CN 201210498809A CN 102942368 A CN102942368 A CN 102942368A
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- bauxite
- grade bauxite
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- propping agent
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Abstract
The invention discloses a method for preparing a high-strength petroleum fracturing propping agent from low-grade bauxite. In the method, low-grade bauxite used as a raw material is treated by a mineral dressing method to increase the aluminum-silicon ratio; and then, the raw material is mixed with auxiliary materials to prepare the high-strength petroleum fracturing propping agent. The method comprises the following steps: (1) selecting a representative low-grade bauxite ore sample, crushing and grinding the raw ore, and increasing the aluminum-silicon ratio of the raw material through an anionic oleic acid collector direct flotation or cationic amine collector reverse flotation method; and (2) grinding the floated bauxite with the increased aluminum-silicon ratio, then mixing with the auxiliary materials according to a certain ratio, further mixing and pulverizing in a jet pulverizing machine, then granulating in a coating machine to obtain a green compact having an appropriate particle size, and sintering the green compact in a rotary kiln to obtain the high-strength petroleum fracturing propping agent. According to the invention, the process is simple and environment-friendly, the low-grade bauxite can be utilized, and the production cost is low.
Description
Technical field
The present invention relates to a kind of production method of using low-grade bauxite to prepare high-strength compress supporting agent for coarse oil, belong to new material technology field.
Background technology
Petroleum fracturing propping agent plays very important effect to oil, gas extraction, is to make the deep layer rock keep the upholder of the state of splitting.During the oil and gas deep mining, high locking pressure deposits of low permeability splits petroliferous strata after fracture treatment, and oil gas compiles from the crack.Enter Filling with propping material in rock crack in company with high-pressure solution, can play make support the crack not stress discharge and closed effect, thereby keep high flow conductivity, make oil gas unimpeded, increase output.
Petroleum fracturing propping agent commonly used has the composite particles of quartz sand, haydite and various resin-coated etc. at present.Wherein the price of quartz sand is the most cheap, and relative density is lower, but the intensity of quartz sand is low, sphericity is poor, percentage of damage is large, thereby has reduced the flow conductivity in crack, is not suitable for especially the high deep-well of locking pressure.And the composite particles of employing resin-coated quartz sand, sphericity is improved, and erosion resistance can reach than high target, even inner quartz sand is crushed, the resin layer that the outside coats can wrap fragment, keeps the flow conductivity in crack.But this shelf life of products is short, and cost is high.
Summary of the invention
The object of the invention is can not directly prepare as raw material for the low-grade bauxite of present complicated ingredient the deficiency of petroleum fracturing propping agent, invents a kind of method that is prepared petroleum fracturing propping agent by low-grade bauxite.
The present invention is prepared high-strength compress supporting agent for coarse oil by low-grade bauxite the technical scheme of method is as follows: adopt low-grade bauxite as raw material, this material composition weight percent is: Al
2O
3: 25~50%; TiO
2: 1~8%; SiO
2: 5~30%, and contain following processing step:
(1) low-grade bauxite is carried out broken ore grinding, grinding fineness is 50%~85%-0.074 millimeter, uses negatively charged ion oleic-acid collecting agent direct flotation or cationic amines collecting agent reverse flotation method, obtains the bauxite product of high aluminium silicon ratio;
(2) the bauxite product with high aluminium silicon ratio carries out again ore grinding, makes its granularity reach 270~48 microns, mixes according to a certain percentage with auxiliary material afterwards, and wherein the weight percent of various auxiliary materials is about 5~20%;
(3) after mixed mixture enters and pulverizes in the micronizer mill, enter granulation in the seed-coating machine, obtain the suitable pellet green compact of granularity, the spherolite diameter is 0.1~1.0 millimeter, the spherolite green compact of making are dried under 150~300 ℃ of temperature, make green compact moisture content<2%;
(4) the pellet green compact after the oven dry drop in the rotary kiln, in control burner, the stove, the temperature of stove tail and rotating speed, sintering time, the type of cooling;
Roasting just can reach qualified petroleum fracturing propping agent product after finishing.
Al in the described bauxite product that obtains high aluminium silicon ratio
2O
3Grade bring up to 40~80% scopes, SiO
2Grade be reduced to 1~10% scope.
The auxiliary material of described step (2) is one or more mixture in SILICA FUME, Manganse Dioxide, titanium dioxide, magnesiumcarbonate, magnesium oxide, zirconium dioxide, the aluminium ash, the weight of each auxiliary material accounts for 5~20% of sample gross weight, wherein in each auxiliary material, SILICA FUME: 0.1~60%; Manganse Dioxide: 0.1%~10%; Titanium dioxide: 0.1%~20%; Magnesiumcarbonate and magnesium oxide: 0.1%~10%; Zirconium dioxide: 0.1%~10%; Aluminium ash: 1%~10%.
The granularity of the material of described micronizer mill after out is 5~100 μ m, and the granularity of seed-coating machine green compact out is 0.1~1.0 mm.
The temperature of the burner of described rotary kiln is 1000~1500 ℃, and the temperature at stove middle part is that 800~1500 ℃, the temperature of stove tail are 500~1000 ℃, and the rotating speed of rotary kiln is 0.3~2 m/h.
Technique of the present invention is simple, and the cost of material of employing is cheap and the wide material sources production cost is low.Utilize two kinds of flotation technologies of direct flotation and reverse flotation to improve first the alumina silica ratio of low-grade bauxite, then use it for the high-intensity petroleum fracturing propping agent of preparation, solved low-grade bauxite because of the too low deficiency that can not directly prepare as raw material propping agent of alumina silica ratio, and utilize positive reverse flotation method to improve alumina silica ratio, the rate of recovery is higher.Pick out the auxiliary material of superior performance by experimental study, greatly increased the properties of propping agent, its product can be applied in the actual production.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Low-grade bauxite after the petroleum fracturing propping agent of the present invention's preparation is improved with alumina silica ratio is as main raw material, as auxiliary material, the weight of each auxiliary material accounts for 5~20% of sample gross weight with materials such as SILICA FUME, Manganse Dioxide, titanium dioxide, magnesiumcarbonate, magnesium oxide, zirconium dioxide, aluminium ashes.
Petroleum fracturing propping agent of the present invention is characterised in that the employing low-grade bauxite as raw material, and its component proportions is: Al
2O
3: 25~60%; TiO
2: 1~8%; SiO
2: 5~30%.
(1) the low-grade bauxite sample ore is carried out broken ore grinding after, making its fineness is 70%~85%-0.074 millimeter, flotation collector is added, two kinds of method for floating have been used at this, the one, the direct flotation method of use negatively charged ion oleic-acid collecting agent, the 2nd, the reverse flotation method of use cationic amines collecting agent, the oleic acid consumption is 100~300g/t, the amine collector consumption is 150~450g/t.Contain Al through the raw material that obtains after the method for floating processing
2O
340~80%, contain SiO
21~10%, the raw material that has improved alumina silica ratio will be for the preparation of high-strength compress supporting agent for coarse oil;
(2) bauxite concentrate that flotation is obtained mixes according to a certain percentage with auxiliary material, and wherein the weight percent of various auxiliary materials is 5~20%;
(4) after mixed mixture enters and pulverizes in the micronizer mill, enter granulation in the seed-coating machine, obtain the suitable pellet green compact of granularity, the spherolite diameter is 0.2~1 millimeter, the spherolite green compact of making are dried under 150~300 ℃ of temperature, make green compact moisture content<1%;
(5) the pellet green compact drop in the rotary kiln, in control burner, the stove, the temperature of stove tail and rotating speed, sintering time, the type of cooling.Roasting just can reach qualified high-strength compress supporting agent for coarse oil product after finishing.
Embodiment 1
1) will contain Al
2O
325~40%, TiO
21~4%, SiO
25~26% low-grade bauxite sample ore carries out broken ore grinding, and grinding fineness is 74%-0.074 millimeter.Add oleic acid 150~240g/t, the bauxite froth product that flotation obtains high aluminium silicon ratio contains Al
2O
342~51%, TiO
22~6%, SiO
22~8%;
2) froth product that obtains of flotation mixes according to a certain percentage with auxiliary material, and the weight percent of auxiliary material is 10%, wherein SILICA FUME in the auxiliary material: 50%; Manganse Dioxide: 5%; Titanium dioxide: 5%; Magnesiumcarbonate and magnesium oxide: 4.5%; Zirconium dioxide: 0.5%; Aluminium ash: 35%.
3) after mixed mixture enters and pulverizes in the micronizer mill, enter dressing and interior granulation, obtain the suitable pellet green compact of granularity.
4) the pellet green compact drop in the rotary kiln, and the temperature at 1500 ℃ of end flue temperatures of control, stove middle part is 800~1500 ℃, 1000 ℃ of stove tail temperature, rotating speed 1 m/h.After finishing, roasting obtains the petroleum fracturing propping agent product.
After testing, each index of product is as follows: ultimate compression strength: 〉=40MPa; Locking pressure: 〉=65MPa; Acid solubility:<4.5%; Particle diameter: 0.40~0.50 mm; Percentage of damage:<3.5%; Sphericity and circularity: 〉=0.8.
Embodiment 2
1) will contain Al
2O
329~51%, TiO
21~2%, SiO
26~28% low-grade bauxite sample ore carries out broken ore grinding, and grinding fineness is 80%-0.074 millimeter.Add amine collector 180~260g/t, the concentrate product that flotation obtains contains Al
2O
342~56%, TiO
21.5~6%, SiO
21~9%;
2) froth product that obtains of flotation mixes according to a certain percentage with auxiliary material, and the weight percent of auxiliary material is 5%, wherein SILICA FUME in the auxiliary material: 45%; Manganse Dioxide: 5%; Titanium dioxide: 5%; Magnesiumcarbonate and magnesium oxide: 4.5%; Zirconium dioxide: 0.5%; Aluminium ash: 40%.
3) after mixed mixture enters and pulverizes in the micronizer mill, enter dressing and interior granulation, obtain the suitable pellet green compact of granularity.
4) the pellet green compact drop in the rotary kiln, and the temperature at 1000 ℃ of end flue temperatures of control, stove middle part is 800 ℃, 500 ℃ of stove tail temperature, rotating speed 1.5 m/h.After finishing, roasting obtains the petroleum fracturing propping agent product.
After testing, each index of product is as follows: ultimate compression strength: 〉=50MPa; Locking pressure: 〉=65MPa; Acid solubility:<4.0%; Particle diameter: 0.45~0.55 mm; Percentage of damage:<3.0%; Sphericity and circularity: 〉=0.9.
Embodiment 3
1) will contain Al
2O
334~60%, TiO
23~7%, SiO
28~30% low-grade bauxite sample ore carries out broken ore grinding, and grinding fineness is 85%-0.074 millimeter.Add oleic collector 200~350g/t, the concentrate product that flotation obtains contains Al
2O
340~60%, TiO
24.5~9%, SiO
24~10%;
2) froth product that obtains of flotation mixes according to a certain percentage with auxiliary material, and the weight percent of auxiliary material is 5%, wherein SILICA FUME in the auxiliary material: 35%; Manganse Dioxide: 5%; Titanium dioxide: 15%; Magnesiumcarbonate and magnesium oxide: 14.5%; Zirconium dioxide: 0.5%; Aluminium ash: 35%.
3) after mixed mixture enters and pulverizes in the micronizer mill, enter dressing and interior granulation, obtain the suitable pellet green compact of granularity;
4) the pellet green compact drop in the rotary kiln, and the temperature at 1300 ℃ of end flue temperatures of control control, stove middle part is 1000 ℃, 700 ℃ of stove tail temperature, rotating speed 0.8 m/h.After finishing, roasting obtains the petroleum fracturing propping agent product.
After testing, each index of product is as follows: ultimate compression strength: 〉=45MPa; Locking pressure: 〉=65MPa; Acid solubility:<4.2%; Particle diameter: 0.50~0.60 mm; Percentage of damage:<3.3%; Sphericity and circularity: 〉=0.9.
Use low-grade bauxite low as its density of petroleum fracturing propping agent of raw material preparation in this inventive method, ultimate compression strength is large, percentage of damage is little, can effectively solve current ultimate compression strength deficiency and the poor problem of flow conductivity, its raw material sources are wide, complete processing is simple, facility investment is little, and energy consumption is little, and cost is low.
Claims (5)
1. method that is prepared high-strength compress supporting agent for coarse oil by low-grade bauxite is characterized in that: adopt low-grade bauxite as raw material, this material composition weight percent is: Al
2O
3: 25~50%; TiO
2: 1~8%; SiO
2: 5~30%, and contain following processing step:
(1) low-grade bauxite is carried out broken ore grinding, grinding fineness is 50%~85%-0.074 millimeter, uses negatively charged ion oleic-acid collecting agent direct flotation or cationic amines collecting agent reverse flotation method, obtains the bauxite product of high aluminium silicon ratio;
(2) the bauxite product with high aluminium silicon ratio carries out again ore grinding, makes its granularity reach 270~48 microns, mixes according to a certain percentage with auxiliary material afterwards, and wherein the weight percent of various auxiliary materials is about 5~20%;
(3) after mixed mixture enters and pulverizes in the micronizer mill, enter granulation in the seed-coating machine, obtain the suitable pellet green compact of granularity, the spherolite diameter is 0.1~1.0 millimeter, the spherolite green compact of making are dried under 150~300 ℃ of temperature, make green compact moisture content<2%;
(4) the pellet green compact after the oven dry drop in the rotary kiln, in control burner, the stove, the temperature of stove tail and rotating speed, sintering time, the type of cooling;
Roasting just can reach qualified petroleum fracturing propping agent product after finishing.
2. a kind of method that is prepared high-strength compress supporting agent for coarse oil by low-grade bauxite according to claim 1 is characterized in that: Al in the described bauxite product that obtains high aluminium silicon ratio
2O
3Grade bring up to 40~80% scopes, SiO
2Grade be reduced to 1~10% scope.
3. a kind of production method that is prepared petroleum fracturing propping agent by low-grade bauxite according to claim 1, it is characterized in that: auxiliary material described step 2) is one or more mixture in SILICA FUME, Manganse Dioxide, titanium dioxide, magnesiumcarbonate, magnesium oxide, zirconium dioxide, the aluminium ash, the weight of each auxiliary material accounts for 5~20% of sample gross weight, wherein in each auxiliary material, SILICA FUME: 0.1~60%; Manganse Dioxide: 0.1%~10%; Titanium dioxide: 0.1%~20%; Magnesiumcarbonate and magnesium oxide: 0.1%~10%; Zirconium dioxide: 0.1%~10%; Aluminium ash: 1%~10%.
4. a kind of production method that is prepared petroleum fracturing propping agent by low-grade bauxite according to claim 1, the granularity that it is characterized in that the material after micronizer mill is out is 5~100 μ m, the granularity of seed-coating machine green compact out is 0.1~1.0 mm.
5. a kind of production method that is prepared petroleum fracturing propping agent by low-grade bauxite according to claim 1, the temperature that it is characterized in that the burner of rotary kiln is 1000~1500 ℃, the temperature at stove middle part is that 800~1500 ℃, the temperature of stove tail are 500~1000 ℃, and the rotating speed of rotary kiln is 0.3~2 m/h.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103288420A (en) * | 2013-05-16 | 2013-09-11 | 陕西科技大学 | Method for preparing fracturing propping agent special for shale gas from fly ash |
CN103525396A (en) * | 2013-10-17 | 2014-01-22 | 西南石油大学 | Method for preparing medium-density high-strength propping agent by utilizing medium-grade and low-grade bauxite |
CN103922710A (en) * | 2014-04-22 | 2014-07-16 | 攀枝花秉扬科技开发有限公司 | Low-density and high-strength ceramic particle and manufacture method thereof |
CN105295889A (en) * | 2014-07-31 | 2016-02-03 | 北京神州卓越石油科技有限公司 | Preparation method of low-density high-strength haydite proppant |
CN110628411A (en) * | 2019-09-24 | 2019-12-31 | 大唐同舟科技有限公司 | Low-density petroleum fracturing propping agent and preparation method thereof |
CN113666730A (en) * | 2021-08-31 | 2021-11-19 | 西南科技大学 | High-strength oil fracturing magnesium aluminum silicate proppant and preparation method thereof |
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CN101012498A (en) * | 2007-02-12 | 2007-08-08 | 李乾宽 | Method for producing high alumina refined powder by using alumyte |
CN102786922A (en) * | 2012-08-23 | 2012-11-21 | 昆明冶金研究院 | Method for preparing high-strength oil fracturing proppant by high-iron bauxite |
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Patent Citations (2)
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CN101012498A (en) * | 2007-02-12 | 2007-08-08 | 李乾宽 | Method for producing high alumina refined powder by using alumyte |
CN102786922A (en) * | 2012-08-23 | 2012-11-21 | 昆明冶金研究院 | Method for preparing high-strength oil fracturing proppant by high-iron bauxite |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103288420A (en) * | 2013-05-16 | 2013-09-11 | 陕西科技大学 | Method for preparing fracturing propping agent special for shale gas from fly ash |
CN103288420B (en) * | 2013-05-16 | 2014-04-16 | 陕西科技大学 | Method for preparing fracturing propping agent special for shale gas from fly ash |
CN103525396A (en) * | 2013-10-17 | 2014-01-22 | 西南石油大学 | Method for preparing medium-density high-strength propping agent by utilizing medium-grade and low-grade bauxite |
CN103922710A (en) * | 2014-04-22 | 2014-07-16 | 攀枝花秉扬科技开发有限公司 | Low-density and high-strength ceramic particle and manufacture method thereof |
CN103922710B (en) * | 2014-04-22 | 2015-03-11 | 攀枝花秉扬科技开发有限公司 | Low-density and high-strength ceramic particle and manufacture method thereof |
CN105295889A (en) * | 2014-07-31 | 2016-02-03 | 北京神州卓越石油科技有限公司 | Preparation method of low-density high-strength haydite proppant |
CN105295889B (en) * | 2014-07-31 | 2019-01-08 | 北京神州卓越石油科技有限公司 | A kind of preparation method of low-density and high-strength ceramsite sand proppant |
CN110628411A (en) * | 2019-09-24 | 2019-12-31 | 大唐同舟科技有限公司 | Low-density petroleum fracturing propping agent and preparation method thereof |
CN110628411B (en) * | 2019-09-24 | 2022-01-11 | 大唐同舟科技有限公司 | Low-density petroleum fracturing propping agent and preparation method thereof |
CN113666730A (en) * | 2021-08-31 | 2021-11-19 | 西南科技大学 | High-strength oil fracturing magnesium aluminum silicate proppant and preparation method thereof |
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Application publication date: 20130227 |