CN102718522B - Method for preparing fracturing propping agent by using rejects - Google Patents
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Abstract
The invention provides a method for preparing fracturing propping agent by using rejects. The method comprises the following steps of: mixing gold ore tailings, Pb-Zn slag, aluminum oxide power and reinforcing agent, adding gum water solution, and grinding, so as to obtain mixed mud; and granulating the mixed mud by a pressure type spray granulator, putting granules into an alumina crucible, and sintering, so as to prepare composite propping agent haycite. According to the method, the idea of a composite material is integrated into the incompact haycite propping agent, so that the fiber (the crystal whisker) required for enhancing the strength and the toughness can be provided in a manner of high-temperature reaction self-generation, and the high-strength, high-toughness, low-density and low-damage rate composite propping agent haycite can be prepared by using two means for enhancing the fiber and the granules, and therefore, a product can be used in a medium-deep level fracturing environment, and the final aim of the production increasing of oil gas can be realized.
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 rejects to prepare 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 oil-gas field belongs to middle deep, requires fracturing propping agents to have high strength, low percentage of damage, to bear the various corrosion in the huge pressure in rock stratum and the ground environment.In the world adopt the alundum goods as in, deep-seated oil gas field fracturing propping agents, though this goods can meet the demands raw material sources difficulty, complete processing complexity, and energy consumption is big, cost is high, and its application is restricted on physicochemical property.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 to improve its comprehensive mechanical property by control chemical ingredients and microstructure under hot conditions, 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 basalt be the furnace charge of main raw material preparation, through fusing, special one-tenth pearl and thermal treatment process, be developed into pyroxene type microcrystal silicon hydrochlorate pearl body.The military patent of Zhousheng (application number: 89102544.8) disclose " a kind of Selid propping agent and manufacture method thereof ", is main raw material with bauxitic clay, through the balling-up of electric arc furnace meltblown, has the ultimate compression strength height, and percentage of damage is low, density moderate with characteristics such as cost is low.Although the propping agent of meltblown method preparation is used in practice to some extent,, prepare ceramsite propping agent with this method and have defectives such as energy consumption height, 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, the non-sintered moulding of organic curing or mix the effect of playing the sand prevention Oil Guide in the fracturing liquid.This series products is not to be truly proppant in high intensity.
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 has defective aspect intensity.
Sintering process is to adopt ceramic raw 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, be major ingredient with bauxitic clay or aluminum oxide, add feldspar, titanium oxide or contain barium carbonate or bar fusing assistant, prepare high-strength low close propping agent, improved 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 bauxitic clay, and this resource to high-quality is a waste greatly, 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, acidproof 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, the prospect that has influenced suitability for industrialized production and applied.
At present, low-density high-strength hangs down the crisp corrosion-resistant main research tendency of propping agent haydite that becomes, for realizing this goal, in the propping agent prescription, introduce different high temperature fusing assistants and optimized the mode of haydite moulding, improved the mechanical property of propping agent to a certain extent, improve 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 discarded slag that both utilized is provided, improve the chemical constitution of propping agent again, optimize the microstructure of haydite, the rejects that utilizes that overcomes stupalith fragility prepares the method for fracturing propping agents.
For achieving the above object, preparation method of the present invention is as follows:
1) gold ore tailing and plumbous zinc ore slag are put into ball mill for dry grinding respectively, cross 120 mesh sieves then respectively;
2) get gold ore tailing after sieving respectively, plumbous zinc ore slag, aluminum oxide powder, toughener, by the gold mine tailings: plumbous zinc ore slag: aluminum oxide powder: toughener=30%～45%: 10%～15%: 30%～45%: 10%～15% mass percent mix compound and compound is put into ball mill to add mass concentration be 10% gummy aqueous solution mixing wet-milling, wet-milling is to utilize the alumina balls masonry to be grinding medium, the control abrading-ball, the mass ratio of compound and 10% the gummy aqueous solution is (2～3): 1: (0.3～0.4), milling time is 0.5h～3h, form mixing mud, mud is crossed 300 mesh sieves;
3) mud after will sieving 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, rate of heating with 5 ℃/min～10 ℃/min is warming up to 1230 ℃ from room temperature, 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, namely get the composite proppant haydite.
Described dry grinding utilizes 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 sponging granulator inlet temperature 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 toughener is barium carbonate.
By the fracturing propping agents that preparation method of the present invention makes, to be formed by matrix phase and wild phase two portions, matrix is by quartz, celsian-felspar and glassy phase, pore phase composite; Wild phase is the corundum of grain refining, generated in-situ not Lay stone, zinc silicate fiber phase, and wherein the mass percent of wild phase is 5～15%, and the mass percent of matrix phase is 85～95%.
The present invention is integrated in the theory of matrix material among the ceramsite propping agent of non-densification, mode with the pyroreaction self-generating provides enhancing toughness reinforcing necessary fiber (whisker), strengthen the compound propping agent haydite that two kinds of means are prepared high-strength and high ductility, low density and LB rate by fiber reinforcement and particle, make this product can be applied in, in the profound pressure break environment, realize the final purpose of frscturing; The present invention also utilizes rejects to be major ingredient in addition, thinking with " adjusting chemical ingredients+optimization microstructure ", by technological operation simple and easy to control, introduce or when utilizing the reaction in self-generating to have fibrous crystals, make fiber and the fine particle of generation between disperse matrix phase, further optimize the concrete grammar that forms fibrous/granular composite ceramic material, " dual disperse " technology is combined with the Ceramic Composite technology, both developed discarded slag, improve the chemical constitution of propping agent again, optimize the microstructure of haydite, overcome the fragility of stupalith, be expected to further improve the over-all properties of propping agent ceramsite material.
Description of drawings
Fig. 1 is to be that major ingredient is in the section SEM of 1400 ℃ of sintered specimens figure with the rejects.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1:
1) gold ore tailing and plumbous zinc ore slag 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 2h crosses 120 mesh sieves then respectively respectively;
2) get the gold ore tailing after sieving, plumbous zinc ore slag, aluminum oxide powder, toughener respectively, by the gold mine tailings: plumbous zinc ore slag: aluminum oxide powder: toughener=30%: 15%: 45%: 10% mass percent mix compound and compound is put into ball mill to add mass concentration be 10% gummy aqueous solution mixing wet-milling, wet-milling is to utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball, compound and 10% the gummy aqueous solution is 2: 1: 0.3, milling time is 0.5h, form mixing mud, mud is crossed 300 mesh sieves;
Described aluminum oxide powder is industrial Alpha-alumina (lapis amiridis), its corundum content＞98%, and the powder grain is through＜10 μ m;
Described toughener is barium carbonate;
3) mud after will sieving adopts the granulation of press spray tablets press, the sponging granulator inlet temperature is 500 ℃, hot-blast furnace temperature is 800 ℃, temperature of outgoing air is 95 ℃, 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, rate of heating with 5 ℃/min is warming up to 1230 ℃ from room temperature, insulation 0.5h～1h, rate of heating with 5 ℃/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, namely get the composite proppant haydite.
As seen from Figure 1, this material matrix is by celsian-felspar, cristobalite principal crystalline phase and a certain amount of pore phase composite, and wild phase is Al
2O
3Phase and Mo Laishi, zinc silicate.This material grains is tiny, is disperse-grain refining structure, and pore is grown, not Lay stone and zinc silicate fiber abrim in the pore.
Table 1 is for being that major ingredient is in the performance index of 1400 ℃ of prepared fracturing propping agents haydite samples with the rejects.
The performance of 1400 ℃ of prepared fracturing propping agents haydite samples of table 1
Embodiment 2:
1) gold ore tailing and plumbous zinc ore slag 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 1h crosses 120 mesh sieves then respectively respectively;
2) get the gold ore tailing after sieving, plumbous zinc ore slag, aluminum oxide powder, toughener respectively, by the gold mine tailings: plumbous zinc ore slag: aluminum oxide powder: toughener=45%: 10%: 30%: 15% mass percent mix compound and compound is put into ball mill to add mass concentration be 10% gummy aqueous solution mixing wet-milling, wet-milling is to utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball, compound and 10% the gummy aqueous solution is 2.5: 1: 0.33, milling time is 3h, form mixing mud, mud is crossed 300 mesh sieves;
Described aluminum oxide powder is industrial Alpha-alumina (lapis amiridis), its corundum content＞98%, and the powder grain is through＜10 μ m;
Described toughener is barium carbonate;
3) mud after will sieving adopts the granulation of press spray tablets press, the sponging granulator inlet temperature is 300 ℃, hot-blast furnace temperature is 600 ℃, temperature of outgoing air is 80 ℃, 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, rate of heating with 8 ℃/min is warming up to 1230 ℃ from room temperature, insulation 0.5h～1h, rate of heating with 6 ℃/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, namely get the composite proppant haydite.
Embodiment 3:
1) gold ore tailing and plumbous zinc ore slag 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 1.5h crosses 120 mesh sieves then respectively respectively;
2) get the gold ore tailing after sieving, plumbous zinc ore slag, aluminum oxide powder, toughener respectively, by the gold mine tailings: plumbous zinc ore slag: aluminum oxide powder: toughener=40%: 12%: 35%: 13% mass percent mix compound and compound is put into ball mill to add mass concentration be 10% gummy aqueous solution mixing wet-milling, wet-milling is to utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball, compound and 10% the gummy aqueous solution is 3: 1: 0.38, milling time is 1h, form mixing mud, mud is crossed 300 mesh sieves;
Described aluminum oxide powder is industrial Alpha-alumina (lapis amiridis), its corundum content＞98%, and the powder grain is through＜10 μ m;
Described toughener is barium carbonate;
3) mud after will sieving adopts the granulation of press spray tablets press, the sponging granulator inlet temperature is 400 ℃, hot-blast furnace temperature is 700 ℃, temperature of outgoing air is 85 ℃, 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, rate of heating with 6 ℃/min is warming up to 1230 ℃ from room temperature, insulation 0.5h～1h, rate of heating with 7 ℃/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, namely get the composite proppant haydite.
Embodiment 4:
1) gold ore tailing and plumbous zinc ore slag 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 crosses 120 mesh sieves then respectively respectively;
2) get the gold ore tailing after sieving, plumbous zinc ore slag, aluminum oxide powder, toughener respectively, by the gold mine tailings: plumbous zinc ore slag: aluminum oxide powder: toughener=35%: 11%: 40%: 14% mass percent mix compound and compound is put into ball mill to add mass concentration be 10% gummy aqueous solution mixing wet-milling, wet-milling is to utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball, compound and 10% the gummy aqueous solution is 2.3: 1: 0.4, milling time is 2h, form mixing mud, mud is crossed 300 mesh sieves;
Described aluminum oxide powder is industrial Alpha-alumina (lapis amiridis), its corundum content＞98%, and the powder grain is through＜10 μ m;
Described toughener is barium carbonate;
3) mud after will sieving adopts the granulation of press spray tablets press, the sponging granulator inlet temperature is 350 ℃, hot-blast furnace temperature is 650 ℃, temperature of outgoing air is 90 ℃, 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, rate of heating with 10 ℃/min is warming up to 1230 ℃ from room temperature, insulation 0.5h～1h, rate of heating with 5 ℃/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, namely get the composite proppant haydite.
The present invention is major ingredient with the rejects, utilizes pyroreaction, the fibrous 3Al of original position self-forming
2O
32SiO
2Mo Laishi and ZnSiO
4The matrix material of granular dispersion consolidatedization of crystal in zinc silicate crystal and the porcelain body, not only have cheap for manufacturing cost, and fibrous not Lay stone has bigger specific surface area and surface energy and granular corundum, cristobalite, the celsian ceramics matrix relies on strong crystal boundary power to combine, fibrous crystals is distributed in corundum on the one hand, cristobalite, between the celsian-felspar particle, form the fiber/particle disperse structure, on the other hand, synthetic corundum crystal tool " grain refining " structure, even dispersion cristobalite, around the crystal such as celsian-felspar, formed 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 and two kinds of rejects of plumbous zinc ore tailings as major ingredient.Waste residue is the inevitable waste that produces in the ore dressing process, has a large capacity and a wide range, and its profile is fine-grained powder powder semisolid, and fineness is generally at 70 orders-160 order, and discharging is piled up loose, does not obtain good development and utilization at present.According to the geologic feature of domestic gold mine output, gold mine waste residue essential mineral is based on quartzy (30%～60%), pyrite (5%～20%), plagioclase (10%～30%), potassium felspar sand (15%～30%), sericite (5%～15%).Plumbous zinc ore slag essential mineral contains components such as a certain amount of Cu, Cd, Hg, Ni, As in addition based on quartzy (30%～45%), potassium felspar sand (10%～20%), pyrite (15%～20%), limonite (5%～10%), rhombspar (5%～10%), diopside (5%～10%), barite (5%～10%).Rejects both provided pyroreaction necessary component, had played the effect of high temperature composite fluxing agent again.Tailings embodies at composition: the characteristics of high silicon, low aluminium, high ferro, potassium, sodium, and in the feature that shows low melting point in nature, efficiently fluxes.The main source of mullite fiber is the SiO in the waste residue under the high temperature
2With the Al in the aluminum oxide powder
2O
3Reaction forms mullite cylinder or fiber, SiO
2Reaction can form fibrous zinc silicate crystal with ZnO, 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 celsian-felspar, cristobalite around, formed the microstructure of dual disperse.The generation of corundum and mullite has been played conclusive effect to proppant strength, and barite and barium carbonate have participated in SiO
2, Al
2O
3, BaO building-up reactions form celsian-felspar, both improved the intensity of haydite and the ability of acid-alkali-corrosive-resisting, reduced the withstand voltage percentage of damage of propping agent again, on the other hand flux component K in the waste residue
2O, Na
2O, CaO, MgO, Fe
2O
3, TiO
2And other trace element etc., can effectively reduce the low eutectic point of compound, the propping agent sintering temperature is reduced, and a spot of glassy phase that forms with other component interactions, be filled in and emit gas or crystalline form because of pyroreaction and transform in the formed pore of volumetric expansion, the raising of the intensity that improves propping agent has been played effectively replenished.
The present invention utilizes rejects, aluminium vanadine, toughener through sintering process, synthetic simultaneously in matrix phase and wild phase by pyroreaction, and make matrix phase " grain refining ", " disperseization ", wild phase and matrix mutually again " disperse ", dual disperse has prepared the composite proppant haydite.Because this material combines the advantage of grain refining stupalith and filamentary material, and make wherein pore mutually also be the disperse attitude evenly to distribute, intensity and the toughness of haydite have been increased on the one hand, effectively reduce 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 rejects 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 rejects as major ingredient, not only can bring into play the waste residue fine size, high silicon, low aluminium, iron, titanium, potassium, sodium component content is big, fusing point is low, the high temperature obvious results advantage of fluxing, can also control pyroreaction by processing condition, make the granular crystal (celsian-felspar of existing high-intensity disperse attitude in the petroleum fracturing propping agent, cristobalite, corundum), have again and strengthen toughness reinforcing fibrous crystals (Mo Laishi, zinc silicate), the two presents disperse-thin brilliant orderly microtexture, thereby effectively improves intensity and the acid fastness of propping agent, 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 rejects, prepares fracturing propping agents with waste residue and not only helps to save natural resource, reduces production costs, and also helps environment protection.
(2) the rejects 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 a large amount of energy consumptions that the raw material ball milling produces effectively.
(3) to have high silicon, low aluminium, iron, titanium foreign matter content big for the performance of the chemical constitution of waste residue and character, and obvious results characteristics that fusing point is low, high temperature is fluxed both provided necessary SiO in the pyroreaction
2, Al
2O
3, ensured 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, when adopting rejects in a large number, introduce the compound enhancing toughner of barium carbonate, make the granular/granular-crystalline structure of existing high-intensity disperse in the petroleum fracturing propping agent-thin crystalline state, the crystalline structure that strengthens toughness reinforcing fiber/granular disperseization is arranged again, thereby effectively improved the microstructure of porcelain body, improved intensity and the acid-resistant corrosion of propping agent, reduced its percentage of damage.
(5) Zhi Bei fracturing propping agents intensity can reach 85MPa～120MPa, 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.
Claims (5)
1. method of utilizing rejects to prepare fracturing propping agents is characterized in that:
1) gold ore tailing and plumbous zinc ore slag are put into ball mill for dry grinding respectively, cross 120 mesh sieves then respectively;
2) get respectively aluminum oxide powder, toughener and sieve after gold ore tailing and plumbous zinc ore slag, by the gold mine tailings: plumbous zinc ore slag: aluminum oxide powder: toughener=30%～45%: 10%～15%: 30%～45%: 10%～15% mass percent mix compound and compound is put into ball mill to add mass concentration be 10% gummy aqueous solution mixing wet-milling, form mixing mud, mud is crossed 300 mesh sieves;
Described toughener is barium carbonate;
3) mud after will sieving 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, rate of heating with 5 ℃/min～10 ℃/min is warming up to 1230 ℃ from room temperature, 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, namely get the composite proppant haydite.
2. the method for utilizing rejects to prepare fracturing propping agents according to claim 1, it is characterized in that: described dry grinding utilizes the alumina balls masonry to be grinding medium, and the mass ratio of control abrading-ball and raw material be (2～3): 1, distinguish ball milling 0.5h～2h.
3. the method for utilizing rejects to prepare fracturing propping agents according to claim 1; it is characterized in that: described sponging granulator inlet temperature is 300 ℃～500 ℃; hot-blast furnace temperature is 600 ℃～800 ℃, and temperature of outgoing air is 80 ℃～95 ℃, and mud pressure is 1.2MPa～1.5Mpa.
4. the method for utilizing rejects to prepare fracturing propping agents according to claim 1, it is characterized in that: described 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), milling time are 0.5h～3h.
5. the method for utilizing rejects to prepare fracturing propping agents according to claim 1, it is characterized in that: described aluminum oxide powder is industrial Alpha-alumina, its corundum content＞98%, the powder grain is through＜10 μ m.
Priority Applications (1)
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| CN105860953A (en) * | 2016-04-14 | 2016-08-17 | 东北大学 | Oil fracturing propping agent and preparation method thereof |
| CN108300453A (en) * | 2017-11-23 | 2018-07-20 | 柳州市柳晶科技股份有限公司 | A kind of ceramsite propping agent prepared using industrial residue |
| CN110467470A (en) * | 2019-07-05 | 2019-11-19 | 青岛理工大学 | A kind of preparation method using electroplating sludge sintered building haydite |
| CN116177883B (en) * | 2023-02-22 | 2023-12-12 | 四川君和环保股份有限公司 | High-strength ceramsite fracturing propping agent and preparation method thereof |
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| CA2785796C (en) * | 2009-12-30 | 2017-06-27 | Schlumberger Canada Limited | Hydraulic fracturing proppant containing inorganic fibers |
| CN102071006B (en) * | 2010-11-22 | 2012-12-05 | 大庆油田有限责任公司 | Petroleum support agent prepared from oil shale waste and preparation method thereof |
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