CN102718532A - Method for preparing composite fracturing proppant by using gold tailings and mullite fiber - Google Patents
Method for preparing composite fracturing proppant by using gold tailings and mullite fiber Download PDFInfo
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- CN102718532A CN102718532A CN2012102013971A CN201210201397A CN102718532A CN 102718532 A CN102718532 A CN 102718532A CN 2012102013971 A CN2012102013971 A CN 2012102013971A CN 201210201397 A CN201210201397 A CN 201210201397A CN 102718532 A CN102718532 A CN 102718532A
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Abstract
The invention relates to a method for preparing composite fracturing proppant by using gold tailings and mullite fiber. The method comprises the steps of: mixing the gold tailings, alumina powder and high-temperature resistant polycrystal mullite chopped fiber, then adding gum water solution into the mixture and evenly mixing; wet grinding and pelleting; putting granules into an alumina crucible and arranging in a silicon carbide rod resistance furnace; heating up to be at 1230 DEG C from the room temperature at the heating speed of 5-10 DEG C/min; carrying out heat preservation for 0.5-1 hour; heating up to be at 1350-1400 DEG C at the heating speed of 5-7 DEG C/min; carrying out the heat preservation for 2-3 hours; naturally cooling along with the furnace and then taking out a product; and finally, sieving by using a sieve of 20-40 meshes so as to obtain the composite fracturing proppant. According to the method, the idea of composite materials is integrated into non-dense ceramic proppant; and the fiber (whisker) required by reinforcing and toughening is provided in a way of assisting high-temperature reaction self generation, so that the composite fracturing proppant which is high in strength and toughness and low in density and damage rate can be prepared by two ways including fiber reinforcement and particulate reinforcement.
Description
Technical field
The present invention relates to a kind of method of utilizing waste material to prepare ceramic composite, particularly a kind of method of utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents.
Background technology
Fracturing propping agents are as an emerging industry, and are not long at China's development time, and its product structure and kind are still far from perfect, and the process scale of industry and level all are in the developmental stage at initial stage.Most of fld belongs to moderate depth, requires fracturing propping agents to have HS, low percentage of damage, to bear the various corrosion in huge pressure in rock stratum and the ground environment.In the world more adopt the alundum goods as in, deep-seated oil gas field fracturing propping agents, though this goods on physicochemical property, can meet the demands, the raw material sources difficulty, complete processing is complicated, and energy consumption is big, cost is high, and its application is restricted.The closed fracturing material of the nonpetroleum deep-well that forms with ceramic sintering method sintering; Be natural siliceous sand, coat in composite particles, glass sphere, the Metal Ball etc., the substitute of low strength propping agent; Have intensity height, low density characteristics, thereby become one of research focus of petrochemical complex material.Current, the subject matter that the fracturing propping agents haydite faces is how under hot conditions, to improve its comprehensive mechanical property through control chemical ingredients and microstructure, effectively reduces the fragility of material, to improve the practical application effect of this material.
Existing propping agent haydite preparation method has meltblown method, organism to coat solidification method, sintering process etc.
Tang Minhui etc. [Research of Support Grains for Oil Well [J]. HarBin Building University's journal; 1995; 28 (4): 73-76] with Irish touchstone be the furnace charge of main raw material preparation,, be developed into pyroxene type microcrystal silicon hydrochlorate pearl body through fusing, special one-tenth pearl and thermal treatment process.Patent discloses " a kind of Selid propping agent and method of manufacture thereof " (characteristics such as Zhousheng is military, and application number: 89102544.8), uses bauxitic clay to be main raw material, through the balling-up of electric arc furnace meltblown, have the ultimate compression strength height, percentage of damage is low, and the moderate and cost of density is low.Although the propping agent of meltblown method preparation is used in reality to some extent,, prepare ceramsite propping agent with this method and have defectives such as energy consumption is high, balling-up is wayward, proppant strength is low, seldom be used at present.
Organism coat solidification method be with organic binder bond as solidifying agent, be raw material with artificial or natural powder, adhesive solidification is unburned to form, though intensity is low, density is little, has certain characteristics.Sun Hu, Wang Yi send out patent (application number 200710188410) " preparation method of low-density propping agent and preparation technology "; Zhou Fujian patent (application number 201010278084) " a kind of fiber composite sand prevention material and preparation method thereof "; Utilize vegetable fibre or organic fibrous material as raw material respectively, organic curing is unburned forms type or mixes the effect of playing the sand prevention Oil Guide in the fracturing liquid.This series products is not to be proppant in high intensity truly.
Have the investigator to prepare fracturing propping agents with FMS-△ G type, FMS-(R) type resin coating method in addition, its product increases aspect crisp subtracting, but obviously aspect intensity, has defective.
Sintering process is to adopt Ceramic Material and traditional ceramic process to prepare the technology of fine and close ceramsite propping agent.The existing many documents of development and the patent report that prepare the oil fracturing ceramsite propping agent with raw mineral materialss such as bauxitic clays.Gao Haili etc. [development of high-strength petroleum fracturing propping agent [J]. pottery, 2006, (10): 43-46] be main raw material with the local two beach bauxitic clays of Flos Bombacis Malabarici, bauxitic clay raw material and high-titanium blast furnace slag, be developed into high-strength petroleum fracturing propping agent.Patent such as Zhao Shiao, Wu Bailin (application number 201010143771.8), " a kind of preparation method who does not have silicon or low-silicon acidproof ceramic fracturing propping agent "; Patents such as Tian Xiaorang (application number 200710168057) " a kind of preparation method of acid-resistant pressing crack supporting agent "; R. patent such as Dien Ke Er, M. Ai Mengzi (application number 200580030660.3) " sintered spherical pellets " etc. adopts sintering process respectively; With bauxitic clay or aluminum oxide is major ingredient; Add feldspar, titanium oxide or contain barium carbonate or bar fusing assistant; Prepare high-strength low close propping agent, improved the intensity and the acid fastness of material.Sintering process still is the main stream approach for preparing propping agent at present.
Prepare propping agent with sintering process; The major ingredient that adopts is a bauxitic clay, and this is a waste greatly to the fine resource, therefore; With solid waste vast scale substitution of Al alumina cheaply, preparation pressure break ceramsite propping agent is the inexorable trend of home and abroad technical progress and development.This has report on the one hand: Li Qing dimension patent (application number 201010552791.0) " a kind of petroleum propping agent that utilizes the oil shale waste preparation and preparation method thereof " has substituted the part bauxitic clay with oil shale waste and has prepared the propping agent that meets GB.Yin Guoxun etc. [utilize industrial solid wastes such as red mud to prepare haydite [J]. Institutes Of Technology Of He'nan's journal (natural science edition), 2008,27 (4): 491-496].Tian Xiaorang patent (application number 200710137758.X) " utilizes red mud to prepare the method for acid-resistant pressing crack supporting agent ".Open and pass magnesium patent (application number 02134274.1) " ceramic slag haydite and preparation method thereof ".Zhai Guanjie etc. [trial-production of high blending flyash sintering ceramsite [J]. flyash .2008, (1): 42-43] manufactured experimently the high blending flyash sintering ceramsite.Zhang Yujun patent (application number 200910015979.9) " a kind of high-strength compress supporting agent for coarse oil and preparation method thereof " utilizes the petroleum fracturing propping agent of the ceramic rod waste material preparation of high alumina content to have high-strength, acid proof characteristics.
The quality of propping agent haydite performance depends on the internal microstructure of product, to the existing understanding fully of this investigator, and has carried out some useful explorations.Lee accounts for firm patent (application number CN201010136972.5) " low-density ceramic proppant and preparation method thereof "; Change molding mode, utilize the ingenious mode of multilayer cladding, synthetic propping agent with nodular enhancement type of inner core and shell; Product performance have been improved; But molding mode is too complicated, handling not strong, has influenced suitability for industrialized production and the prospect of applying.
At present; Low-density high-strength hangs down the crisp corrosion-resistant main research tendency of propping agent haydite that becomes, and for realizing this goal, in the propping agent prescription, has introduced different high temperature fusing assistants and has optimized the mode of haydite moulding; Improved the mechanical property of propping agent to a certain extent; Improve the acid resistance and the salt tolerance of material, however, still can not fundamentally solve the shortcoming of ceramsite propping agent mechanical property relatively poor (fragility is bigger).
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and means, a kind of method of utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents is provided.Can prepare the compound fracturing propping agents of high-strength and high ductility, low density and LB rate by preparation method of the present invention, make this product can be applied in, in the profound pressure break environment, realize the purpose of frscturing.
For achieving the above object, the technical scheme that the present invention adopts is:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, cross 120 mesh sieves then respectively;
2) gold ore tailing after sieving 40%～55% by mass percentage, 30%～45% aluminum oxide powder and 10%～15% resistant to elevated temperatures polycrystalline Lay stone chopped strand do not join in the ball mill after mixing; In ball mill, add mass concentration again and be 10% gummy aqueous solution mixing wet-milling and form mixing mud, mud is crossed 300 mesh sieves;
3) the back mud that will sieve adopts the granulation of press spray tablets press, and the spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 5 ℃/min～10 ℃/min; Insulation 0.5h～1h; Rate of heating with 5 ℃/min～7 ℃/min is warming up to 1350 ℃～1400 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
Described step 1) dry grinding is to utilize the alumina balls masonry to be grinding medium, and the mass ratio of control abrading-ball and raw material is (2～3): 1, and difference ball milling 0.5h～2h.
Described step 2) wet-milling is to utilize the alumina balls masonry to be grinding medium, and the mass ratio of control abrading-ball, compound and the gummy aqueous solution is (2～3): l: (0.3～0.4), grind 0.5h～3h.
Described step 3) granulation: the sponging granulator EAT is 300 ℃～500 ℃, and hot-blast furnace temperature is 600 ℃～800 ℃, and temperature of outgoing air is 80 ℃～95 ℃, and mud pressure is 1.2MPa～1.5MPa.
Described aluminum oxide powder is industrial Alpha-alumina (lapis amiridis), its corundum content＞98%, and the powder grain is through＜10 μ m.
Described resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃.
Institute of the present invention synthetic is the composite proppant haydite of tool grain refining and disperseization, and it is made up of matrix phase and wild phase two portions, and matrix is mutually mainly by quartz, lime feldspar and a spot of glassy phase, pore phase composite; Wild phase is the corundum of grain refining, the mullite fiber and the generated in-situ not Lay mineral wool phase of introducing.The moity of material than (wt%) is: wild phase 5-15%, matrix phase 85-95%.
The present invention utilizes trade waste-gold ore tailing to be major ingredient; With the thinking of " adjustment chemical ingredients+optimizations microstructure ", when having fibrous crystals through the reaction in self-generating, the fine particle that makes fiber and generation from the disperse matrix mutually between the concrete grammar of the fibrous/granular composite ceramic material of further optimization formation; " dual disperse " technology is combined with the Ceramic Composite technology; Both develop the depleted slag, improved the chemical constitution of propping agent again, optimized the microstructure of haydite; Overcome the fragility of stupalith, be expected to further improve the over-all properties of propping agent ceramsite material.
Embodiment
Embodiment 1:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and raw material is 2: 1, and ball milling 0.5h～2h crosses 120 mesh sieves then respectively respectively;
2) gold ore tailing after sieving 40% by mass percentage, 45% aluminum oxide powder and 15% resistant to elevated temperatures polycrystalline not Lay stone chopped strand put into ball mill; Adding mass concentration again and be 10% gummy aqueous solution mixing utilizes the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is 2: l: 0.3; Grind 0.5h～3h and form mixing mud, mud is crossed 300 mesh sieves;
Wherein, aluminum oxide powder is that industrial Alpha-alumina is a lapis amiridis, its corundum content＞98%, and the powder grain is through＜10 μ m; Resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃;
3) will sieving afterwards, mud adopts the granulation of press spray tablets press; The sponging granulator EAT is 500 ℃; Hot-blast furnace temperature is 800 ℃, and temperature of outgoing air is 95 ℃, and mud pressure is 1.2MPa; The spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 5 ℃/min; Insulation 0.5h～1h; Rate of heating with 5 ℃/min is warming up to 1350 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
Embodiment 2:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and raw material is 2.5: 1, and ball milling 0.5h～2h crosses 120 mesh sieves then respectively respectively;
2) gold ore tailing after sieving 55% by mass percentage, 30% aluminum oxide powder and 15% resistant to elevated temperatures polycrystalline not Lay stone chopped strand put into ball mill; Adding mass concentration again and be 10% gummy aqueous solution mixing utilizes the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is 2.5: l: 0.35; Grind 0.5h～3h and form mixing mud, mud is crossed 300 mesh sieves;
Wherein, aluminum oxide powder is that industrial Alpha-alumina is a lapis amiridis, its corundum content＞98%, and the powder grain is through＜10 μ m; Resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃;
3) will sieving afterwards, mud adopts the granulation of press spray tablets press; The sponging granulator EAT is 300 ℃; Hot-blast furnace temperature is 600 ℃, and temperature of outgoing air is 80 ℃, and mud pressure is 1.4MPa; The spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 8 ℃/min; Insulation 0.5h～1h; Rate of heating with 6 ℃/min is warming up to 1380 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
Embodiment 3:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and raw material is 3: 1, and ball milling 0.5h～2h crosses 120 mesh sieves then respectively respectively;
2) gold ore tailing after sieving 50% by mass percentage, 40% aluminum oxide powder and 10% resistant to elevated temperatures polycrystalline not Lay stone chopped strand put into ball mill; Adding mass concentration again and be 10% gummy aqueous solution mixing utilizes the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is 3: l: 0.38; Grind 0.5h～3h and form mixing mud, mud is crossed 300 mesh sieves;
Wherein, aluminum oxide powder is that industrial Alpha-alumina is a lapis amiridis, its corundum content＞98%, and the powder grain is through＜10 μ m; Resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃;
3) will sieving afterwards, mud adopts the granulation of press spray tablets press; The sponging granulator EAT is 400 ℃; Hot-blast furnace temperature is 700 ℃, and temperature of outgoing air is 88 ℃, and mud pressure is 1.3MPa; The spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 6 ℃/min; Insulation 0.5h～1h; Rate of heating with 7 ℃/min is warming up to 1360 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
Embodiment 4:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and raw material is 2.3: 1, and ball milling 0.5h～2h crosses 120 mesh sieves then respectively respectively;
2) gold ore tailing after sieving 45% by mass percentage, 43% aluminum oxide powder and 12% resistant to elevated temperatures polycrystalline not Lay stone chopped strand put into ball mill; Adding mass concentration again and be 10% gummy aqueous solution mixing utilizes the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is 2.3: l: 0.33; Grind 0.5h～3h and form mixing mud, mud is crossed 300 mesh sieves;
Wherein, aluminum oxide powder is that industrial Alpha-alumina is a lapis amiridis, its corundum content＞98%, and the powder grain is through＜10 μ m; Resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃;
3) will sieving afterwards, mud adopts the granulation of press spray tablets press; The sponging granulator EAT is 350 ℃; Hot-blast furnace temperature is 650 ℃, and temperature of outgoing air is 84 ℃, and mud pressure is 1.5MPa; The spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 7 ℃/min; Insulation 0.5h～1h; Rate of heating with 5 ℃/min is warming up to 1390 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
Embodiment 5:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and raw material is 2.8: 1, and ball milling 0.5h～2h crosses 120 mesh sieves then respectively respectively;
2) gold ore tailing after sieving 52% by mass percentage, 35% aluminum oxide powder and 13% resistant to elevated temperatures polycrystalline not Lay stone chopped strand put into ball mill; Adding mass concentration again and be 10% gummy aqueous solution mixing utilizes the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is 2.8: l: 0.4; Grind 0.5h～3h and form mixing mud, mud is crossed 300 mesh sieves;
Wherein, aluminum oxide powder is that industrial Alpha-alumina is a lapis amiridis, its corundum content＞98%, and the powder grain is through＜10 μ m; Resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃;
3) will sieving afterwards, mud adopts the granulation of press spray tablets press; The sponging granulator EAT is 450 ℃; Hot-blast furnace temperature is 750 ℃, and temperature of outgoing air is 92 ℃, and mud pressure is 1.2MPa; The spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 10 ℃/min; Insulation 0.5h～1h; Rate of heating with 5 ℃/min is warming up to 1370 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
Embodiment 6:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and raw material is 3: 1, and ball milling 0.5h～2h crosses 120 mesh sieves then respectively respectively;
2) gold ore tailing after sieving 50% by mass percentage, 36% aluminum oxide powder and 14% resistant to elevated temperatures polycrystalline not Lay stone chopped strand put into ball mill; Adding mass concentration again and be 10% gummy aqueous solution mixing utilizes the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is 3: l: 0.4; Grind 0.5h～3h and form mixing mud, mud is crossed 300 mesh sieves;
Wherein, aluminum oxide powder is that industrial Alpha-alumina is a lapis amiridis, its corundum content＞98%, and the powder grain is through＜10 μ m; Resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃;
3) will sieving afterwards, mud adopts the granulation of press spray tablets press; The sponging granulator EAT is 380 ℃; Hot-blast furnace temperature is 680 ℃, and temperature of outgoing air is 90 ℃, and mud pressure is 1.5MPa; The spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 9 ℃/min; Insulation 0.5h～1h; Rate of heating with 7 ℃/min is warming up to 1400 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
The present invention is major ingredient with the gold ore tailing, when introducing not the Lay mineral wool, utilizes pyroreaction, the fibrous 3Al of original position self-forming
2O
32SiO
2The matrix material of granular dispersion consolidatedization of crystal in Lay stone crystal and the porcelain body not; Not only have cheap for manufacturing cost; And fibrous not Lay stone has bigger specific surface area and surface energy relies on strong crystal boundary power to combine with granular corundum, cristobalite, lime feldspar ceramic matrix, and fibrous crystals is distributed between corundum, cristobalite, the lime feldspar particle on the one hand, forms the fiber/particle disperse structure; On the other hand; Synthetic corundum crystal tool " grain refining " structure, even dispersion crystal such as cristobalite, lime feldspar around, form the stack of particle/particle secondary disperse." dual disperse " caused the formation of fiber/granular compound disperse structure, effectively improved the microstructure of porcelain body, intensity and the toughness that improves porcelain body played conclusive effect, thereby the over-all properties of this material is greatly improved.
In the ceramsite propping agent prescription, introduce and at high temperature fully to react the chemical composition that forms fibrous crystals; With it as necessary initial feed; Make fibrous crystals and new formation between the granular crystal through pyroreaction, synthesized " dual disperse " microstructural matrix material.Because each different under uniform temp, environment and condition, forming mutually; Cause fiber reinforcement and particle to reach mutually between the pore phase and have good stress consistency and wettability; Effectively improve and optimized the microstructure of haydite, this comprehensive mechanical performance is significantly improved.
The present invention prepares petroleum fracturing propping agent with gold ore tailing as major ingredient.Tailings is the inevitable waste residue that produces during gold is produced, and has a large capacity and a wide range, and does not obtain good development and utilization at present.Geologic feature according to domestic gold output; Gold mine waste residue essential mineral is main with quartzy (30%～60%), pyrite (5%～20%), plagioclase (10%～30%), potassium felspar sand (15%～30%), sericite (5%～15%), and chemical constitution is generally with SiO
2(40%～60%), Al
2O
3(15%～25%), Fe
2O
3(2%～10%), TiO
2(0～2%), K
2O (3%～8%), Na
2O oxide compounds such as (2%～5%) form to exist, and profile is that the fine-grained powder powder is semi-solid, and discharging is piled up loose, and granularity is at 70 orders～160 orders (between the 0.22mm～0.097mm).Gold ore tailing both provided pyroreaction necessary component, had played the effect of high temperature composite fluxing agent again.Tailings embodies on composition: the characteristics of high silicon, low aluminium, high ferro, potassium, sodium, and in the characteristic that shows lower melting point in nature, efficiently fluxes.The main source of mullite fiber is the SiO in the waste residue under outside introducing and the high temperature
2With the Al in the aluminum oxide powder
2O
3Reaction forms mullite cylinder or fiber, and fiber phase/particle phase/pore has constituted the microstructure of disperse attitude mutually.Non-α-Al
2O
3Be transformed into the particulate corundum of wild phase, the corundum wild phase also be thin crystalline substance-disperse attitude be distributed in lime feldspar, cristobalite around, formed the microstructure of dual disperse.The generation of corundum and mullite has been played conclusive effect to proppant strength.Be flux component K on the other hand in the tailings
2O, Na
2O, CaO, MgO, Fe
2O
3, TiO
2Deng; Can effectively reduce the low eutectic point of compound; The propping agent sintering temperature is reduced; And with a spot of glassy phase that other component interactions form, be filled in because of pyroreaction and emit gas or crystalline form transforms in the formed pore of volumetric expansion, the intensity that improves propping agent has been played has effectively replenished.
The present invention utilizes gold ore tailing, aluminum oxide powder, the Lay mineral wool is not through sintering process; Synthetic simultaneously through pyroreaction in matrix phase and wild phase; And make matrix phase " grain refining ", " disperseization ", wild phase and matrix mutually once more " disperse ", dual disperse has prepared the composite proppant haydite.Because this material combines the advantage of grain refining stupalith and filamentary material; And make pore wherein also be disperse attitude uniform distribution mutually; The intensity and the toughness of haydite have been increased on the one hand; Effectively reduce the density and the breakage rate of material on the other hand, make this comprehensive mechanical performance obtain further raising.In addition, on raw material, introduce gold ore tailing cheaply in a large number, reduced firing temperature, in burning till fast, realized grain refining and disperseization, reduced production cost simultaneously.The present invention does not change existing technology, does not increase any equipment, and the technical indicator of its product and use properties meet oil and gas industry standard SY/T5108-2006 " fracturing propping agents performance index and evaluation test method " fully.
The present invention prepares compound petroleum fracturing propping agent with gold ore tailing as major ingredient; Not only can bring into play gold ore tailing fine size, high silicon, low aluminium, iron, titanium, potassium, sodium component content is big; Obvious results advantage that fusing point is low, high temperature is fluxed; Can also make the granular crystal of existing high-intensity disperse attitude (lime feldspar, cristobalite, corundum) in the petroleum fracturing propping agent through processing condition control pyroreaction, have again to strengthen toughness reinforcing fibrous crystals (Mo Laishi); The two presents disperse-thin brilliant orderly microtexture, thus effectively improve propping agent intensity and acid fastness, reduce its percentage of damage.Form the proppant material of excellent performance.
Effect of the present invention is embodied in:
(1) main raw material of the present invention is the trade waste of inevitable discharging in the ore dressing process, prepares fracturing propping agents with gold ore tailing and not only helps to practice thrift natural resource, reduces production costs, and helps environment protection.
(2) the tailings raw material is mainly micron-size spherical particles, compares with natural mineral, and raw material need not to use high-power crusher in crushing, and batch mixing is even between the each component, has reduced the mass energy consumption that the raw material ball milling is produced effectively.
(3) mineralogical chemistry of gold ore tailing is formed that performance has high silicon with character, is hanged down aluminium, iron, titanium foreign matter content is big, and obvious results characteristics that fusing point is low, high temperature is fluxed both provided necessary SiO in the pyroreaction
2, Al
2O
3Deng component, supplied with antiflux component K again
2O, Na
2O, Fe
2O
3, TiO
2, CaO, MgO etc., reduce production cost.
(4) theory with matrix material is guidance; Introduced not Lay mineral wool; Make the corundum crystal of existing high-intensity disperse in the fracturing propping agents-thin crystalline state constitute particle/particulate disperse structure, the fiber/particle disperse structure that strengthens toughness reinforcing fibrous disperseization is arranged again, dual disperse has effectively improved the microstructure of porcelain body; Improve the intensity and the acid-resistant corrosion of propping agent, reduce its percentage of damage.
(5) the fracturing propping agents intensity of preparation can reach 95MPa～135MPa, has intensity height, light weight, good characteristic such as high temperature resistant, corrosion-resistant, in can be used as, the fracturing propping agents of deep-seated oil gas field.
Table 1 is the performance index of major ingredient in 1400 ℃ of prepared fracturing propping agents haydite samples for the introducing fiber and with the gold ore tailing.
The performance of 1400 ℃ of prepared fracturing propping agents haydite samples of table 1
Claims (6)
1. method of utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents is characterized in that:
1) gold ore tailing and aluminum oxide powder are put into ball mill for dry grinding respectively, cross 120 mesh sieves then respectively;
2) gold ore tailing after sieving 40%～55% by mass percentage, 30%～45% aluminum oxide powder and 10%～15% resistant to elevated temperatures polycrystalline Lay stone chopped strand do not join in the ball mill after mixing; In ball mill, add mass concentration again and be 10% gummy aqueous solution mixing wet-milling and form mixing mud, mud is crossed 300 mesh sieves;
3) the back mud that will sieve adopts the granulation of press spray tablets press, and the spheroidal particle that granulation forms is crossed 18 orders and 30 mesh sieves, the screenings particle between two sieves is collected waited to burn;
4) particle to be burnt is put into alumina crucible, and place in the globars resistance furnace, be warming up to 1230 ℃ from room temperature with the rate of heating of 5 ℃/min～10 ℃/min; Insulation 0.5h～1h; Rate of heating with 5 ℃/min～7 ℃/min is warming up to 1350 ℃～1400 ℃, and insulation 2h～3h is with taking out behind the stove naturally cooling; Cross 20 orders～40 mesh sieves, promptly get the composite fracturing propping agent.
2. the method for utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents according to claim 1; It is characterized in that: described step 1) dry grinding is to utilize the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball and raw material is (2～3): 1, and difference ball milling 0.5h～2h.
3. the method for utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents according to claim 1; It is characterized in that: described step 2) wet-milling is to utilize the alumina balls masonry to be grinding medium; The mass ratio of control abrading-ball, compound and the gummy aqueous solution is (2～3): l: (0.3～0.4), grind 0.5h～3h.
4. the method for utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents according to claim 1; It is characterized in that: described step 3) granulation: the sponging granulator EAT is 300 ℃～500 ℃; Hot-blast furnace temperature is 600 ℃～800 ℃; Temperature of outgoing air is 80 ℃～95 ℃, and mud pressure is 1.2MPa～1.5MPa.
5. the method for utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents according to claim 1; It is characterized in that: described aluminum oxide powder is industrial Alpha-alumina (lapis amiridis); Its corundum content＞98%, the powder grain is through＜10 μ m.
6. the method for utilizing gold ore tailing and mullite fiber to prepare compound fracturing propping agents according to claim 1 is characterized in that: described resistant to elevated temperatures polycrystalline not Lay stone chopped strand use temperature is 1350-1450 ℃.
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| CN112300776A (en) * | 2020-11-03 | 2021-02-02 | 洛阳赛罗帕陶瓷科技有限公司 | Fracturing propping agent with corundum-anorthite as main crystal phase and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585698A (en) * | 2009-07-03 | 2009-11-25 | 陕西科技大学 | Method for preparing porcelain granules by using fly ash |
| WO2011081545A1 (en) * | 2009-12-30 | 2011-07-07 | Schlumberger Canada Limited | Hydraulic fracturing proppant containing inorganic fibers |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585698A (en) * | 2009-07-03 | 2009-11-25 | 陕西科技大学 | Method for preparing porcelain granules by using fly ash |
| WO2011081545A1 (en) * | 2009-12-30 | 2011-07-07 | Schlumberger Canada Limited | Hydraulic fracturing proppant containing inorganic fibers |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300776A (en) * | 2020-11-03 | 2021-02-02 | 洛阳赛罗帕陶瓷科技有限公司 | Fracturing propping agent with corundum-anorthite as main crystal phase and preparation method thereof |
| CN112300776B (en) * | 2020-11-03 | 2022-05-31 | 洛阳赛罗帕陶瓷科技有限公司 | Fracturing propping agent with corundum-anorthite as main crystal phase and preparation method thereof |
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