CN103288426B - A kind of method utilizing industrial waste to prepare the special fracturing propping agents of shale gas - Google Patents
A kind of method utilizing industrial waste to prepare the special fracturing propping agents of shale gas Download PDFInfo
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- CN103288426B CN103288426B CN201310204233.9A CN201310204233A CN103288426B CN 103288426 B CN103288426 B CN 103288426B CN 201310204233 A CN201310204233 A CN 201310204233A CN 103288426 B CN103288426 B CN 103288426B
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- shale gas
- powder
- kaolin
- propping agents
- fracturing propping
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
A kind of method utilizing industrial waste to prepare the special fracturing propping agents of shale gas, waste residue powder is formed by sieving with airflow milling fragmentation after flyash and/or calcined coal gangue, weigh in proportion and put into mixer mix with waste residue powder and kaolin, polycrystalline silica flour, through granulation balling-up, particle after balling-up is put into crucible, and sinter in electric furnace and take out after naturally cooling, obtain the special fracturing propping agents of shale gas.The method not only raw material sources is extensive, and improves the microstructure of porcelain body, and firing temperature is low, and firing period is short, save energy, low-carbon environment-friendly, improves the over-all properties of product; The propping agent density of preparation is low, and intensity is high, has the good characteristics such as high temperature resistant, corrosion-resistant, and in can be, deep layer shale gas field provides the fracturing material of better performances.
Description
Technical field
The present invention relates to a kind of method preparing fracturing propping agents, particularly a kind of method utilizing industrial waste to prepare the special fracturing propping agents of shale gas.
Background technology
Fracturing propping agents are as an emerging industry, 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 are all in the developmental stage at initial stage.Most of oil gas field belongs to middle deep, requires that fracturing propping agents have high strength, low percentage of damage, to bear the various corrosion in the huge pressure in rock stratum and ground environment.In the world adopt alundum goods as in, deep-seated oil gas field fracturing propping agents, although this goods can meet the demands on physicochemical property, raw material sources difficulty, complete processing is complicated, and energy consumption is large, cost is high, makes it apply and is restricted.Fracturing material is closed with the nonpetroleum deep-well of ceramic firing method sintering, be in natural siliceous sand, covered composite yarn particle, glass sphere, Metal Ball etc., the substitute of low strength propping agent, there is high, the low density feature of intensity, thus become one of study hotspot of petrochemical complex material.Current, the subject matter that fracturing propping agents haydite faces how to improve its comprehensive mechanical property by control chemical composition and microstructure under the high temperature 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, Coated with Organic Matter solidification method, sintering process etc.
Chinese patent 89102544.8 discloses " a kind of Selid propping agent and manufacture method thereof ", is main raw material with bauxitic clay, and through the balling-up of electric arc furnace meltblown, have ultimate compression strength high, percentage of damage is low, medium density and the feature such as cost is low.Although the standby propping agent of meltblown legal system is applied in practice to some extent, prepare ceramsite propping agent by the method and there is the defects such as energy consumption is high, balling-up is wayward, proppant strength is low, be seldom used at present.
Coated with Organic Matter solidification method is using organic binder bond as solidifying agent, and with artificial or natural powder for raw material, adhesive solidification is unburned to be formed, although intensity is low, density is little, has certain feature.Chinese patent 200710188410 discloses " preparation method of low-density propping agent and preparation technology ", Chinese patent 201010278084 discloses " a kind of fiber composite sand control material and preparation method thereof ", utilize vegetable fibre or organic fibrous material as raw material respectively, organic curing non-sintered shaping or mix in fracturing liquid the effect playing sand prevention Oil Guide.This series products is not proppant in high intensity truly.
Sintering process is the technology adopting ceramic raw material and traditional ceramic process to prepare fine and close ceramsite propping agent.The development preparing oil fracturing ceramsite propping agent with raw mineral materialss such as bauxitic clays has many documents and patent report.Gao Haili etc. " development [J] of high-strength petroleum fracturing propping agent. pottery; 2006; (10): 43-46 ", with Flos Bombacis Malabarici local two beach bauxitic clays, bauxitic clay raw material and high-titanium blast furnace slag for main raw material, be developed into high-strength petroleum fracturing propping agent; Chinese patent 201010143771.8 discloses " a kind of preparation method without silicon or low-silicon acidproof ceramic fracturing propping agent ", adopt sintering process respectively, with bauxitic clay or aluminum oxide for major ingredient, add feldspar, titanium oxide or contain barium carbonate or bar fusing assistant, prepare high-strength low close propping agent, improve intensity and the acid fastness of material.Sintering process is still prepare the main stream approach of propping agent at present.
Prepare propping agent with sintering process, the major ingredient of employing is bauxitic clay, and this is a waste greatly to the resource of high-quality, and therefore, with low cost waste material vast scale substitution of Al alumina, preparation pressure break ceramsite propping agent is the inexorable trend of home and abroad technological progress and development.This has been reported on the one hand: Chinese patent 201010552791.0 discloses " a kind of petroleum propping agent utilizing oil shale waste to prepare and preparation method thereof " instead of part bauxitic clay with oil shale waste and prepare the propping agent meeting GB.Zhai Guanjie etc. " trial-production [J] of high blending flyash sintering ceramsite. flyash .2008, (1): 42-43 ", manufactured experimently high blending flyash sintering ceramsite.But apply normal pressure-sintered technique means in its preparation process, sintering temperature is higher.
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.Chinese patent CN201010136972.5 discloses " low-density ceramic proppant and preparation method thereof ", change molding mode, utilize the ingenious mode of multilayer cladding, synthesis has the propping agent of the nodular enhancement type of inner core and shell, improve product performance, but it is not molding mode is too complicated, handling strong, the prospect that have impact on suitability for industrialized production He apply.
At present, low-density high-strength is corrosion-resistant becomes the main research tendency of propping agent haydite, for realizing this goal, different high temperature fusing assistants is introduced in propping agent formula, improve the mechanical property of propping agent to a certain extent, improve acid resistance and the salt tolerance of material, however, still fundamentally can not solve the shortcoming that ceramsite propping agent mechanical property is poor, sintering temperature is higher.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing industrial waste to prepare the special fracturing propping agents of shale gas, the method raw material sources are extensive, and improve the microstructure of porcelain body, firing temperature is low, firing period is short, low-carbon environment-friendly, and production cost is low, production process is simple and easy to control, constant product quality.
For achieving the above object, the technical solution used in the present invention comprises the following steps:
1) by flyash and/or calcined coal gangue, material must be calcined;
2) calcining material is carried out fragmentation, obtain waste residue powder; Kaolin is carried out fragmentation, obtains kaolin powder;
3) by mass percentage, the waste residue powder of 93% ~ 96.5%, the kaolin powder of 3% ~ 6%, the polycrystalline silica flour of 0.5% ~ 1% are mixed, obtains compound;
4) by compound granulation balling-up in nodulizer, the particle being a granulated into ball formation crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into crucible, and be placed in electric furnace, and at 1330 DEG C ~ 1380 DEG C, be incubated 1h ~ 1.5h, take out after naturally cooling to room temperature with stove, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas.
Described step 1) is when calcined fine coal powder and/or coal gangue, and controlling calcining temperature is 830 ~ 860 DEG C, insulation 30 ~ 40min.
The step 2 stated) middle calcining is expected and kaolin adopts cyclonic jet mill to carry out fragmentation, controls the material size≤3mm of cyclonic jet mill respectively, product grading < 5 μm, air pressure >=0.8Mpa.
Described step 2) when fragmentation calcining material and kaolin, control the material size≤3mm of cyclonic jet mill respectively, product grading < 5 μm, air pressure >=0.8Mpa.
Polycrystalline silica flour in described step 3) is active silica flour, the massfraction more than 95% of Si in active silica flour, and can pass through 325 mesh sieves.
Crucible in described step 5) adopts alumina crucible, and electric furnace is globars resistance furnace.
It is rise to 150 DEG C with the rate of heating of 3 DEG C/min ~ 5 DEG C/min from room temperature that described step 5) treating in electric furnace burns particle, insulation 5 ~ 10min, is then warming up to 1330 DEG C ~ 1380 DEG C with the rate of heating of 5 DEG C/min ~ 10 DEG C/min.
Compared with prior art, beneficial effect of the present invention is:
1) main raw material of the present invention is trade waste-flyash and/or coal gangue, not only contributes to saving natural resource, increases economic efficiency, and reduces production cost, and is conducive to environment protection, make secondary resource obtain recycling.
2) calcined fine coal powder and/or coal gangue can reduce loss on ignition, improve the Al in flyash and/or coal gangue
2o
3content and activity, have low silicon, high alumina, iron, titanium foreign matter content are large, active substance is many, and fusing point low and high temperature is fluxed the feature of Be very effective, and the polycrystalline silica flour in addition introduced, two aspect actings in conjunction effectively reduce the firing temperature of propping agent haydite.Polycrystalline silica flour has fine size, active large feature, forms low eutectic point on the one hand, make ceramisite sintered temperature be reduced to 1330 ~ 1380 DEG C under high temperature together with flyash or coal gangue, on the other hand silica flour oxidizable formation SiO
2particle, can with the high reactivity Al in major ingredient
2o
3particle generation solid state reaction forms 3Al
2o
32SiO
2not Lay stone primary crystal, and then the Al in induction major ingredient
2o
3and SiO
2original position autoreaction forms fibrous 3Al
2o
32SiO
2the formation of Mo Laishi, Mo Laishi improves the microtexture of porcelain body, effectively improves intensity and the acid fastness of propping agent, reduces its percentage of damage, the proppant material of forming property excellence.
3) product (granularity 20 ~ 40 order) performance made by preparation method of the present invention is: volume density≤1.50g/cm
3; Volume density≤2.72g/cm
3; 52MPa locking pressure percentage of damage 2.0 ~ 4.5%; 69MPa locking pressure percentage of damage 5.0 ~ 8.5%; Acid resistance≤5%, has the low characteristic such as close, high-strength, high temperature resistant, corrosion-resistant, in can be used as, the special fracturing propping agents of deep layer shale gas.
Further, the present invention rises to 150 DEG C with 3 DEG C/min ~ 5 DEG C/min rate of heating from room temperature, and the object of insulation 5 ~ 10min is the moisture of fully discharging in base substrate.
Embodiment
Embodiment 1:
1) calcined by flyash, calcining temperature is 830 DEG C, and insulation 40min, must calcine material;
2) calcining material is put into cyclonic jet mill fragmentation, form calcining material fines, 325 mesh sieves crossed by calcining material fines, obtain waste residue powder; Kaolin is put into cyclonic jet mill fragmentation, form kaolin fines, 325 mesh sieves crossed by kaolin fines, obtain kaolin powder;
3) by mass percentage, the waste residue powder of 93%, the kaolin powder of 6%, the polycrystalline silica flour of 1% are put into mixer and mixed, obtains compound;
4) by compound granulation balling-up in nodulizer, the particle that granulation is formed crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into alumina crucible, and be placed in globars resistance furnace, 150 DEG C are risen to from room temperature with the rate of heating of 3 DEG C/min, insulation 5min, rise to 1330 DEG C with the rate of heating of 5 DEG C/min, insulation 1.5h, takes out with after stove naturally cooling, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas.
Embodiment 2:
1) by calcined coal gangue, calcining temperature is 840 DEG C, and insulation 38min, must calcine material;
2) calcining material is put into cyclonic jet mill fragmentation, form calcining material fines, 325 mesh sieves crossed by calcining material fines, obtain waste residue powder; Kaolin is put into cyclonic jet mill fragmentation, form kaolin fines, 325 mesh sieves crossed by kaolin fines, obtain kaolin powder;
3) by mass percentage, the waste residue powder of 94.1%, the kaolin powder of 5%, the polycrystalline silica flour of 0.9% are put into mixer and mixed, obtains compound;
4) by compound granulation balling-up in nodulizer, the particle that granulation is formed crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into alumina crucible, and be placed in globars resistance furnace, 150 DEG C are risen to from room temperature with the rate of heating of 3 DEG C/min, insulation 6min, rise to 1340 DEG C with the rate of heating of 6 DEG C/min, insulation 1.4h, takes out with after stove naturally cooling, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas.
Embodiment 3:
1) flyash and coal gangue are calcined respectively, calcining temperature is 845 DEG C, insulation 35min, obtains flyash calcining material and calcined coal gangue material respectively;
2) flyash is calcined material and put into cyclonic jet mill fragmentation, form flyash calcining material fines, 325 mesh sieves crossed by flyash calcining material fines, obtain flyash waste residue powder; Calcined coal gangue material is put into cyclonic jet mill fragmentation, and form calcined coal gangue material fines, 325 mesh sieves crossed by calcined coal gangue material fines, obtain coal gangue waste residue powder; Kaolin is put into cyclonic jet mill fragmentation, form kaolin fines, 325 mesh sieves crossed by kaolin fines, obtain kaolin powder;
3) by mass percentage, the mixture of the flyash waste residue powder of 95.3% and colliery powder waste residue powder, the kaolin powder of 4%, the polycrystalline silica flour of 0.7% are put into mixer and mixed, obtains compound; Wherein, the mixture of flyash waste residue powder and colliery powder waste residue powder is that the flyash waste residue powder of 1:2 and colliery powder waste residue powder mix by mass ratio;
4) by compound granulation balling-up in nodulizer, the particle that granulation is formed crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into alumina crucible, and be placed in globars resistance furnace, 150 DEG C are risen to from room temperature with the rate of heating of 4 DEG C/min, insulation 8min, rise to 1350 DEG C with the rate of heating of 8 DEG C/min, insulation 1.3h, takes out with after stove naturally cooling, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas.
Embodiment 4:
1) be the flyash of 1:1 and the calcining of coal gangue mixture by mass ratio, calcining temperature is 850 DEG C, and insulation 32min, must calcine material;
2) calcining material is put into cyclonic jet mill fragmentation, form calcining material fines, 325 mesh sieves crossed by calcining material fines, obtain waste residue powder; Kaolin is put into cyclonic jet mill fragmentation, form kaolin fines, 325 mesh sieves crossed by kaolin fines, obtain kaolin powder;
3) the waste residue powder of 96.4%, the kaolin powder of 3%, the polycrystalline silica flour of 0.6% are put into mixer and mixed, obtain compound;
4) by compound granulation balling-up in nodulizer, the particle that granulation is formed crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into alumina crucible, and be placed in globars resistance furnace, 150 DEG C are risen to from room temperature with the rate of heating of 4 DEG C/min, insulation 9min, rise to 1370 DEG C with the rate of heating of 9 DEG C/min, insulation 1.2h, takes out with after stove naturally cooling, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas.
Embodiment 5:
1) calcined by flyash, calcining temperature is 860 DEG C, and insulation 30min, must calcine material;
2) calcining material is put into cyclonic jet mill fragmentation, form calcining material fines, 325 mesh sieves crossed by calcining material fines, obtain waste residue powder; Kaolin is put into cyclonic jet mill fragmentation, form kaolin fines, 325 mesh sieves crossed by kaolin fines, obtain kaolin powder;
3) by mass percentage, the waste residue powder of 96.5%, the kaolin powder of 3%, the polycrystalline silica flour of 0.5% are put into mixer and mixed, obtains compound;
4) by compound granulation balling-up in nodulizer, the particle that granulation is formed crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into alumina crucible, and be placed in globars resistance furnace, 150 DEG C are risen to from room temperature with the rate of heating of 5 DEG C/min, insulation 10min, rise to 1380 DEG C with the rate of heating of 10 DEG C/min, insulation 1h, takes out with after stove naturally cooling, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas.
The present invention is to the performance index of the special fracturing propping agents of shale gas obtained by above embodiment 1-5 according to SY/T5108-2006, and " fracturing propping agents performance test recommend method " is tested, and test result is as shown in table 1:
The performance index of the special fracturing propping agents of shale gas (20 ~ 40 mesh sieve) that table 1 embodiment 1-5 is obtained
In above-described embodiment 1-5, step 1) is when calcined fine coal powder and/or coal gangue, control material size≤3mm, product grading < 5 μm, air pressure >=0.8Mpa, polycrystalline silica flour in step 3) is active silica flour, the massfraction more than 95% of Si in activate micro powder, and can 325 mesh sieves be passed through.
Present method utilizes the waste-coal gangue in thermal power generation trade waste-flyash and/or coal mining to optimize propping agent chemical constitution.The method has not only developed flyash, Coal Gangue Resource, raw material sources are extensive, and with the high reactivity needed for high temperature solid state reaction for starting point, be chemically active induction factor with polycrystalline silica flour, make use of flyash fully, activity in coal gangue, original position autoreaction synthesizes not Lay mineral wool, improve the microstructure of porcelain body, firing temperature is low, firing period is short, low-carbon environment-friendly, production process is simple and easy to control, constant product quality, low-density and high-strength petroleum fracturing propping agent can be produced, for in, deep layer shale gas field provides the fracturing material of better performances.
Claims (3)
1. utilize industrial waste to prepare a method for the special fracturing propping agents of shale gas, it is characterized in that, comprise the following steps:
1) by flyash and/or calcined coal gangue, material must be calcined;
2) calcining material is carried out fragmentation, obtain waste residue powder; Kaolin is carried out fragmentation, obtains kaolin powder;
3) by mass percentage, the waste residue powder of 93% ~ 96.5%, the kaolin powder of 3% ~ 6%, the polycrystalline silica flour of 0.5% ~ 1% are mixed, obtains compound;
4) by compound granulation balling-up in nodulizer, the particle being a granulated into ball formation crosses 18 order ~ 30 mesh sieves, and the screenings powder collection between sieving two becomes to be waited to burn particle;
5) will wait that burning particle puts into crucible, and be placed in electric furnace, and at 1330 DEG C ~ 1380 DEG C, be incubated 1h ~ 1.5h, take out after naturally cooling to room temperature with stove, cross 20 order ~ 40 mesh sieves, obtain the special fracturing propping agents of shale gas;
Described step 5) to burn particle be rise to 150 DEG C with the rate of heating of 3 DEG C/min ~ 5 DEG C/min from room temperature to treating in electric furnace, insulation 5 ~ 10min, is then warming up to 1330 DEG C ~ 1380 DEG C with the rate of heating of 5 DEG C/min ~ 10 DEG C/min;
Described step 3) in polycrystalline silica flour be active silica flour, wherein, the massfraction more than 95% of Si in active silica flour, and can 325 mesh sieves be passed through;
Described step 5) in crucible adopt alumina crucible, electric furnace is globars resistance furnace.
2. the method utilizing industrial waste to prepare the special fracturing propping agents of shale gas according to claim 1, is characterized in that: described step 1) when calcined fine coal powder and/or coal gangue, controlling calcining temperature is 830 ~ 860 DEG C, insulation 30 ~ 40min.
3. the method utilizing industrial waste to prepare the special fracturing propping agents of shale gas according to claim 1, it is characterized in that: described step 2) middle calcining is expected and kaolin adopts cyclonic jet mill to carry out fragmentation, control the material size≤3mm of cyclonic jet mill respectively, product grading < 5 μm, air pressure >=0.8Mpa.
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CN116177881B (en) * | 2023-02-22 | 2023-11-28 | 四川君和环保股份有限公司 | Ultralow-density ceramsite fracturing propping agent and preparation method thereof |
CN117757461B (en) * | 2023-12-18 | 2024-07-23 | 四川君和环保股份有限公司 | Ceramsite fracturing propping agent with low acid solubility and preparation method thereof |
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