CN105131934A - Double-layer high-strength fracturing propping agent and preparing method thereof - Google Patents
Double-layer high-strength fracturing propping agent and preparing method thereof Download PDFInfo
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- CN105131934A CN105131934A CN201510645034.0A CN201510645034A CN105131934A CN 105131934 A CN105131934 A CN 105131934A CN 201510645034 A CN201510645034 A CN 201510645034A CN 105131934 A CN105131934 A CN 105131934A
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 71
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 69
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 58
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002994 raw material Substances 0.000 claims description 76
- 239000011257 shell material Substances 0.000 claims description 62
- 239000004927 clay Substances 0.000 claims description 49
- 239000010410 layer Substances 0.000 claims description 44
- 239000011230 binding agent Substances 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 29
- HIGRAKVNKLCVCA-UHFFFAOYSA-N alumine Chemical compound C1=CC=[Al]C=C1 HIGRAKVNKLCVCA-UHFFFAOYSA-N 0.000 claims description 26
- 239000003245 coal Substances 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 22
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 10
- 239000011247 coating layer Substances 0.000 claims description 9
- 229920002401 polyacrylamide Polymers 0.000 claims description 9
- 239000010695 polyglycol Substances 0.000 claims description 5
- 229920000151 polyglycol Polymers 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 abstract description 13
- 239000002253 acid Substances 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 229910001570 bauxite Inorganic materials 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 2
- XUIMIQQOPSSXEZ-NJFSPNSNSA-N silicon-30 atom Chemical compound [30Si] XUIMIQQOPSSXEZ-NJFSPNSNSA-N 0.000 abstract 1
- 230000006378 damage Effects 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- 239000007789 gas Substances 0.000 description 12
- 238000000498 ball milling Methods 0.000 description 11
- 238000007906 compression Methods 0.000 description 11
- 230000006835 compression Effects 0.000 description 11
- 238000005469 granulation Methods 0.000 description 11
- 230000003179 granulation Effects 0.000 description 11
- 238000002156 mixing Methods 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- -1 shale Substances 0.000 description 9
- 239000006004 Quartz sand Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000012216 screening Methods 0.000 description 7
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 6
- 238000009818 secondary granulation Methods 0.000 description 5
- 238000005086 pumping Methods 0.000 description 4
- 239000011435 rock Substances 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 208000010392 Bone Fractures Diseases 0.000 description 2
- 206010017076 Fracture Diseases 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
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- 208000014674 injury Diseases 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
- C09K8/805—Coated proppants
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a double-layer high-strength fracturing propping agent and a preparing method thereof and belongs to the technical field of oil (gas) extraction auxiliaries. The fracturing propping agent comprises a ceramic inner core and a silicon nitride ceramic shell wrapped on the surface of the ceramic inner core. The proportion of the diameter of the ceramic inner core and the thickness of the silicon nitride ceramic shell is 5-10:1. The ceramic inner core is mainly prepared from, by mass, 40%-50% of bauxite, 40%-50% of shale and 0-10% of gangue. The silicon nitride ceramic shell is mainly prepared from, by mass, 60%-70% of silicon nitride and 30%-40% of bauxite. The double-layer high-strength fracturing propping agent has the advantage of high tensile strength, the low breaking rate, low apparent density, the high corrosion resistance capability and the like, the breaking rate is smaller than 6% under the condition of 103 Mpa, the acid solubility is smaller than 2%, and the double-layer high-strength fracturing propping agent is particularly suitable for development of deep well and ultra-deep well oil and gas fields.
Description
Technical field
The invention belongs to oil recovery (gas) auxiliary agent technical field, be specifically related to a kind of double-layer high strength fracturing propping agents, also relate to a kind of preparation method of double-layer high strength fracturing propping agents simultaneously.
Background technology
In oil, gas extraction process, waterfrac treatment has become the important means of exploitation.Particularly the condition of storage of China's oil Sweet natural gas has features such as burying deeply, locking pressure is high, rate of permeation is low; In Oil/gas Well deep mining process, high locking pressure deposits of low permeability is after fracture treatment, Oil gas-containing rock layer is split, oil gas collects from the passage of cracking initiation, fluid is now needed to inject rock basic unit, to exceed the pressure of formation fracture intensity, make generation crack in rock stratum around pit shaft, form the passage that has high flow conductivity.Open in order to crack can be kept, oil gas product can produce to ground smoothly, petroleum propping agent being entered together with high-pressure solution stratum is filled in rock crack, the distribution of propping agent in crack decides the flow conductivity in crack, and after pressure break completes, crack can close on the propping agent of filling, therefore propping agent plays the closed dual role of supporting crack and crackle preventing, crack can be made to keep high flow conductivity, make oil gas unimpeded, increase yield.
Fracturing propping agents conventional at present have the particle etc. of quartz sand, haydite and resin coating.Wherein, the price of quartz sand is the most cheap, and relative density is low, constructability pumping, but the intensity of quartz sand is low, degree of sphericity is poor, percentage of damage is high, thus reduces the flow conductivity in crack, is not suitable for the deep-well that locking pressure is high especially.After quartz sand resin coating, degree of sphericity makes moderate progress, and resistant to breakage ability increases substantially, and flow conductivity is better than quartz sand, but still lower than haydite.With the ceramsite propping agent that aluminium vanadine manufactures for major ingredient, degree of sphericity, resistant to breakage ability and flow conductivity are all good than quartz sand, widely adopt by dark Oil/gas Well.But the volume density of haydite is larger than quartz sand, higher requirement is proposed to pumping conditions and of the fracturing fluid performance, increases difficulty of construction; Easily accumulation is caused in fracturing process, extremely unfavorable to water conservancy diversion, thus affect later stage fuel-displaced effect, and simultaneously high to pumping power requirement, large to the wearing and tearing of pipeline.
By contrast, low-density propping agent has good voidage, and it is easier to carry, and can greatly reduce of the fracturing fluid viscosity, reduce the injury to pipeline and pump, even can realize clean fracturing, effectively reduce difficulty of construction and cost for oil production; Low-density propping agent water conservancy diversion lapse rate is lower in addition, the oil recovery effect that can produce.Therefore the exploitation of low-density propping agent becomes the direction of propping agent research.
In prior art, CN101787270B discloses a kind of low-density ceramic proppant, with bauxitic clay and coal gangue for inner core, with bauxitic clay and trimanganese tetroxide for shell, balling-up sinters, and obtain low-density ceramsite, the diameter of described inner core is 0.2 ~ 0.3mm, the particle diameter of described ball is 0.6 ~ 0.95mm, and in described inner core, the weight ratio of bauxitic clay and coal gangue is 20 ~ 80:80 ~ 20; In described shell, the weight ratio of bauxitic clay and trimanganese tetroxide is 90 ~ 97:10 ~ 3.Gained ceramsite propping agent has high, the low density feature of intensity, but adopt the mixture of trimanganese tetroxide and bauxitic clay to form shell, increase rate for the reduction of density, intensity is little, percentage of damage is high simultaneously, resistance to corrosion is weak, can't meet the requirement of high locking pressure, the use of low seepage flow reservoir.
Summary of the invention
The object of this invention is to provide a kind of double-layer high strength fracturing propping agents, solve the feature that existing fracturing propping agents ultimate compression strength is low, percentage of damage is high, volume density is high, resistance to corrosion is weak.
Second object of the present invention is to provide a kind of preparation method of double-layer high strength fracturing propping agents.
In order to realize above object, the technical solution adopted in the present invention is:
A kind of double-layer high strength fracturing propping agents, comprise ceramic core and the silicon nitride ceramics shell being coated on ceramic core surface, the ratio of described ceramic core diameter and silicon nitride ceramics outer casing thickness is 5 ~ 10:1;
Described ceramic core is made primarily of the core raw material of following mass percent: bauxitic clay 40% ~ 50%, shale 40% ~ 50%, coal gangue 0 ~ 10%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 60% ~ 70%, bauxitic clay 30% ~ 40%.
Double-layer high strength fracturing propping agents of the present invention, comprise ceramic core and the silicon nitride ceramics shell being coated on ceramic core surface, ceramic core is made primarily of bauxitic clay, shale and coal gangue, and density is low; Silicon nitride ceramics shell is made primarily of silicon nitride and bauxitic clay, and intensity is high; Gained double-layer high strength fracturing propping agents have the advantages such as ultimate compression strength is high, percentage of damage is low, volume density is low, resistance to corrosion is strong, percentage of damage < 6% under 103Mpa condition, acid solubility < 2%, is specially adapted to the exploitation of deep-well and ultra deep well oil-gas field.
The granularity of described double-layer high strength fracturing propping agents is 40 ~ 70 orders.
Preferably, described ceramic core is made primarily of the core raw material of following mass percent: bauxitic clay 45% ~ 50%, shale 40% ~ 45%, coal gangue 5 ~ 10%.
In described core raw material, bauxitic clay used is low bauxitic clay, and in described low bauxitic clay, the mass content of aluminum oxide is not higher than 50%; In described shell material raw material, bauxitic clay used is alumine, and in described alumine, the mass content of aluminum oxide is not less than 70%.Preferably, in low bauxitic clay, the mass content of aluminum oxide is 40% ~ 50%; In described alumine, the mass content of aluminum oxide is 70% ~ 80%.
Preferably, the specification requirement of each component raw material used is in table 1.
The specification requirement of each component raw material of table 1
Described silicon nitride is alpha silicon nitride or beta silicon nitride.
Preferably, described ceramic core is made up of the core raw material of binding agent and following mass percent: bauxitic clay 40% ~ 50%, shale 40% ~ 50%, coal gangue 0 ~ 10%; Described silicon nitride ceramics shell is made up of the shell material raw material of binding agent and following mass percent: silicon nitride 60% ~ 70%, bauxitic clay 30% ~ 40%.Preparation method comprises: the core raw material of powdery adds binding agent and to granulate to obtain inner core blank; The shell material raw material of powdery adds binding agent, is that core secondary is granulated and formed coating layer, rear roasting and get final product on inner core blank surface with inner core blank.
Described binding agent to be mass concentration be 0.1% ~ 1.0% polyacrylamide solution, cmc soln or polyglycol solution.
Double-layer high strength fracturing propping agents of the present invention, comprise the silicon nitride ceramics shell of low-density ceramic core and high strength, it is advantageous that:
1. silicon nitride is a kind of stupalith of high strength, and it has the performances such as heatproof, withstand voltage, acid and alkali-resistance, and its ultimate compression strength is very high simultaneously, greatly can improve the ultimate compression strength of propping agent and reduce percentage of damage; The ultimate compression strength of product of the present invention can reach 103MPa, and percentage of damage < 6% is specially adapted to the frac job of oil-gas field deep-well and ultra deep well.
2. each feed composition mechanism of action is: core raw material adopts low bauxitic clay, shale, coal gangue, the Al when high-temperature calcination in bauxitic clay and shale
2o
3, SiO
2generate the ultimate compression strength that the bar-shaped mullite crystalline phase with some strength can improve propping agent, meanwhile, the carbon in coal gangue can produce hole of holding one's breath under high-temperature calcination, significantly reduces the volume density of propping agent.Utilize silicon nitride to do case material, utilize Al in itself high strength and alumine
2o
3, SiO
2the corundum generating more high strength improves the ultimate compression strength of propping agent mutually.The ceramic shell that silicon nitride is formed simultaneously has very strong resistance to acids and bases, reduces the acid solubility of propping agent.The case material that silicon nitride is at high temperature formed has good surface smoothness and degree of sphericity, effectively can improve the flow conductivity of propping agent and reduce the turbidity of propping agent.
3. double-layer high strength fracturing propping agents of the present invention, detect according to SY/T5108-2014 standard-required, the volume density of 40/70 order fracturing propping agents is 1.50g/cm
3below, volume density is 2.50g/cm
3below, the percentage of damage under 86Mpa, 103Mpa pressure is respectively 1.5%, 5.0%, and resistance to compression grade can reach 15K, meet exploitation of oil-gas field requirement completely, and volume density is far below industry standard.Meanwhile, fracturing propping agents surface smoothness is good, sphericity is high, and flow conductivity significantly promotes, and lower volume density can reduce the use to guanidine glue in pressing crack construction, easier pumping, can effectively reduce pressure break cost.
A preparation method for above-mentioned double-layer high strength fracturing propping agents, comprises the following steps:
1) get the bauxitic clay of formula ratio, shale, colliery powder be broken into fine powder, be mixed to get core raw material; Silicon nitride, the bauxite powder of getting formula ratio are broken into fine powder, are mixed to get shell material raw material, for subsequent use;
2) by step 1) gained core raw material adds binding agent, inner core blank of granulating to obtain;
3) by step 1) gained shell material raw material adds binding agent, with step 2) gained inner core blank is that core is granulated, form coating layer on inner core blank surface, obtain work in-process;
4) get step 3) gained work in-process dry after carry out roasting, cool and get final product.
Step 1) in, fine powder used meets 500 mesh screen residue≤3% (mass percent).The preparation method of described core raw material or shell material raw material is: first each component raw material is crushed to below 5mm (preferably 1 ~ 5mm) respectively, after distinguishing ball milling 5 ~ 8h again, cross 500 mesh sieves, the fineness to powder reaches 500 mesh screen residue≤3% (mass percent); Press formula ratio mixing afterwards, to obtain final product.
Described binding agent to be mass concentration be 0.1% ~ 1.0% polyacrylamide solution, cmc soln or polyglycol solution.Described binding agent is the aqueous solution that mass concentration is 0.1% ~ 1.0%.
Step 2) in, the mass ratio of described core raw material and binding agent is 100:8 ~ 10; Step 3) in, the mass ratio of described shell material raw material and binding agent is 100:8 ~ 12.
Step 3) in, obtain work in-process with 35 ~ 65 object sieved through sieve after granulating.
Step 4) in, the temperature of described oven dry is 100 ~ 200 DEG C.
Step 4) in, the temperature of described roasting is 1300 ~ 1400 DEG C, and the time of roasting is not less than 6h.Preferably, the temperature of described roasting is 1350 ~ 1400 DEG C, and the time of roasting is 6 ~ 8h.
Step 4) in, obtain finished product with 40 ~ 70 object sieved through sieve after cooling.General, sieve half-finished screen cloth larger than the mesh size of screening finished product, mainly because high-temperature roasting lower volume is shunk, moisture loss also can cause volume-diminished; Such screening mode can ensure high yield rate.
The preparation method of double-layer high strength fracturing propping agents of the present invention, the core raw material comprising powdery adds binding agent granulation (once granulating) and obtains inner core blank, the shell material raw material of powdery adds binding agent, be that core secondary is granulated at inner core blank surface formation coating layer with inner core blank, rear roasting; Adopt double-deck agglomeration technique, obtain the silicon nitride ceramics shell of low-density ceramic core and high strength; In preparation process, more easily control inner core and outer field ratio and performance; Gained double-layer high strength fracturing propping agents, degree of sphericity is high, and quality is good, and percentage of damage is low, and has higher ultimate compression strength and lower density; Preparation process is brief, and starting material are taken conveniently, and processing parameter is controlled, is suitable for large-scale industrial production.
Further, double-layer high strength fracturing propping agents of the present invention and preparation method thereof, core raw material have employed low-grade bauxite and shale is main raw material, significantly can reduce the production cost of propping agent; Also add coal gangue simultaneously, solve comprehensive utilization of resources problem, there is good economic and social benefit.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment 1 gained double-layer high strength fracturing propping agents;
Fig. 2 is the microstructure sectional view of embodiment 1 gained double-layer high strength fracturing propping agents.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
The double-layer high strength fracturing propping agents of the present embodiment, as shown in Figure 1, comprise ceramic core 1 and the silicon nitride ceramics shell 2 being coated on ceramic core 1 surface, the ratio of the diameter of described ceramic core 1 and the thickness of silicon nitride ceramics shell 2 is 7:1;
Described ceramic core is made primarily of the core raw material of following mass percent: low bauxitic clay 45%, shale 45%, coal gangue 10%; In described low bauxitic clay, the mass content of aluminum oxide is 50%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 60%, alumine 40%.In described alumine, the mass content of aluminum oxide is 70%;
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, comprises the following steps:
1) get low bauxitic clay, shale, coal gangue first distinguish (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 8h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained bauxitic clay, shale, coal gangue fine powder mixing and stirring are obtained core raw material, for subsequent use;
Get silicon nitride, alumine first distinguishes (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 8h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained silicon nitride, alumine fine powder mixing and stirring is obtained shell material raw material, for subsequent use;
2) using step 1) to add mass concentration be that the polyacrylamide solution of 0.1% is as binding agent (mass ratio of core raw material and binding agent is 100:10) to gained core raw material, granulation on tablets press (once granulating), obtains inner core blank;
3) using step 1) to add mass concentration be that the polyacrylamide solution of 0.1% is as binding agent (mass ratio of shell material raw material and binding agent is 100:11) to gained shell material raw material, with step 2) gained inner core blank is core granulation on tablets press (secondary granulation), form coating layer on inner core blank surface, adopt 35 ~ 65 eye mesh screens to sieve to obtain work in-process;
4) step 3 is got) gained work in-process 100 DEG C of oven dry, then under 1360 DEG C of conditions after roasting 8h, are cooled to room temperature, adopt 40 ~ 70 eye mesh screens screenings to get product.
The microstructure sectional view of the present embodiment gained double-layer high strength fracturing propping agents as shown in Figure 2.Gained propping agent is cut open from centre by Fig. 2, observes the picture obtained under the microscope.As can be seen from Figure 2, gained double-layer high strength fracturing propping agents are subsphaeroidal, and degree of sphericity is high, epigranular; The structure double-deck as we can see from the figure, color and the inner color at edge are had any different, and display material is different, and small pore can also be seen in centre, and entirety reduces the density of propping agent.
Embodiment 2
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, and comprise ceramic core 1 and the silicon nitride ceramics shell 2 being coated on ceramic core 1 surface, the ratio of the diameter of described ceramic core 1 and the thickness of silicon nitride ceramics shell 2 is 5:1;
Described ceramic core is made primarily of the core raw material of following mass percent: low bauxitic clay 50%, shale 45%, coal gangue 5%; In described low bauxitic clay, the mass content of aluminum oxide is 40%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 70%, alumine 30%.In described alumine, the mass content of aluminum oxide is 80%;
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, comprises the following steps:
1) get low bauxitic clay, shale, coal gangue first distinguish (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 7h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained bauxitic clay, shale, coal gangue fine powder mixing and stirring are obtained core raw material, for subsequent use;
Get silicon nitride, alumine first distinguishes (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 7h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained silicon nitride, alumine fine powder mixing and stirring is obtained shell material raw material, for subsequent use;
2) using step 1) to add mass concentration be that the polyacrylamide solution of 0.1% is as binding agent (mass ratio of core raw material and binding agent is 100:8) to gained core raw material, granulation on tablets press (once granulating), obtains inner core blank;
3) using step 1) to add mass concentration be that the polyacrylamide solution of 0.1% is as binding agent (mass ratio of shell material raw material and binding agent is 100:12) to gained shell material raw material, with step 2) gained inner core blank is core granulation on tablets press (secondary granulation), form coating layer on inner core blank surface, adopt 35 ~ 65 eye mesh screens to sieve to obtain work in-process;
4) step 3 is got) gained work in-process 120 DEG C of oven dry, then under 1380 DEG C of conditions after roasting 7h, are cooled to room temperature, adopt 40 ~ 70 eye mesh screens screenings to get product.
Embodiment 3
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, and comprise ceramic core 1 and the silicon nitride ceramics shell 2 being coated on ceramic core 1 surface, the ratio of the diameter of described ceramic core 1 and the thickness of silicon nitride ceramics shell 2 is 10:1;
Described ceramic core is made primarily of the core raw material of following mass percent: low bauxitic clay 47%, shale 43%, coal gangue 10%; In described low bauxitic clay, the mass content of aluminum oxide is 45%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 65%, alumine 35%.In described alumine, the mass content of aluminum oxide is 75%;
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, comprises the following steps:
1) get low bauxitic clay, shale, coal gangue first distinguish (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 6h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained bauxitic clay, shale, coal gangue fine powder mixing and stirring are obtained core raw material, for subsequent use;
Get silicon nitride, alumine first distinguishes (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 6h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained silicon nitride, alumine fine powder mixing and stirring is obtained shell material raw material, for subsequent use;
2) using step 1) to add mass concentration be that the polyacrylamide solution of 0.1% is as binding agent (mass ratio of core raw material and binding agent is 100:9) to gained core raw material, granulation on tablets press (once granulating), obtains inner core blank;
3) using step 1) to add mass concentration be that the polyacrylamide solution of 0.1% is as binding agent (mass ratio of shell material raw material and binding agent is 100:10) to gained shell material raw material, with step 2) gained inner core blank is core granulation on tablets press (secondary granulation), form coating layer on inner core blank surface, adopt 35 ~ 65 eye mesh screens to sieve to obtain work in-process;
4) step 3 is got) gained work in-process 150 DEG C of oven dry, then under 1360 DEG C of conditions after roasting 8h, are cooled to room temperature, adopt 40 ~ 70 eye mesh screens screenings to get product.
Embodiment 4
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, and comprise ceramic core 1 and the silicon nitride ceramics shell 2 being coated on ceramic core 1 surface, the ratio of the diameter of described ceramic core 1 and the thickness of silicon nitride ceramics shell 2 is 7:1;
Described ceramic core is made primarily of the core raw material of following mass percent: low bauxitic clay 50%, shale 50%; In described low bauxitic clay, the mass content of aluminum oxide is 45%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 60%, alumine 40%.In described alumine, the mass content of aluminum oxide is 70%;
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, comprises the following steps:
1) get low bauxitic clay, shale first distinguishes (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 6h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained bauxitic clay, shale fine powder mixing and stirring is obtained core raw material, for subsequent use;
Get silicon nitride, alumine first distinguishes (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 6h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained silicon nitride, alumine fine powder mixing and stirring is obtained shell material raw material, for subsequent use;
2) using step 1) to add mass concentration be that the cmc soln of 1.0% is as binding agent (mass ratio of core raw material and binding agent is 100:8) to gained core raw material, granulation on tablets press (once granulating), obtains inner core blank;
3) using step 1) to add mass concentration be that the cmc soln of 1.0% is as binding agent (mass ratio of shell material raw material and binding agent is 100:10) to gained shell material raw material, with step 2) gained inner core blank is core granulation on tablets press (secondary granulation), form coating layer on inner core blank surface, adopt 35 ~ 65 eye mesh screens to sieve to obtain work in-process;
4) step 3 is got) gained work in-process 180 DEG C of oven dry, then under 1400 DEG C of conditions after roasting 6h, are cooled to room temperature, adopt 40 ~ 70 eye mesh screens screenings to get product.
Embodiment 5
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, and comprise ceramic core 1 and the silicon nitride ceramics shell 2 being coated on ceramic core 1 surface, the ratio of the diameter of described ceramic core 1 and the thickness of silicon nitride ceramics shell 2 is 10:1;
Described ceramic core is made primarily of the core raw material of following mass percent: low bauxitic clay 43%, shale 47%, coal gangue 10%; In described low bauxitic clay, the mass content of aluminum oxide is 50%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 70%, alumine 30%.In described alumine, the mass content of aluminum oxide is 80%;
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, comprises the following steps:
1) get low bauxitic clay, shale, coal gangue first distinguish (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 6h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained bauxitic clay, shale, coal gangue fine powder mixing and stirring are obtained core raw material, for subsequent use;
Get silicon nitride, alumine first distinguishes (through jaw crusher) and be crushed to below 5mm, be placed in ball mill ball milling 6h again, fineness to powder reaches 500 mesh screen residue≤3%, by formula ratio, gained silicon nitride, alumine fine powder mixing and stirring is obtained shell material raw material, for subsequent use;
2) using step 1) to add mass concentration be that the polyglycol solution of 0.5% is as binding agent (mass ratio of core raw material and binding agent is 100:10) to gained core raw material, granulation on tablets press (once granulating), obtains inner core blank;
3) using step 1) to add mass concentration be that the polyglycol solution of 0.5% is as binding agent (mass ratio of shell material raw material and binding agent is 100:10) to gained shell material raw material, with step 2) gained inner core blank is core granulation on tablets press (secondary granulation), form coating layer on inner core blank surface, adopt 35 ~ 65 eye mesh screens to sieve to obtain work in-process;
4) step 3 is got) gained work in-process 200 DEG C of oven dry, then under 1380 DEG C of conditions after roasting 7h, are cooled to room temperature, adopt 40 ~ 70 eye mesh screens screenings to get product.
Experimental example
This experimental example is according to SY/T5108-2014 standard, and carry out Performance Detection to embodiment 1-5 gained double-layer high strength fracturing propping agents, detected result sees the following form 2.
The performance test results of table 2 embodiment 1 ~ 5 gained double-layer high strength fracturing propping agents
| Performance index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Volume density (g/cm 3) | 1.43 | 1.47 | 1.50 | 1.49 | 1.48 |
| Volume density (g/cm 3) | 2.41 | 2.45 | 2.50 | 2.50 | 2.46 |
| Circularity | 0.91 | 0.91 | 0.90 | 0.90 | 0.90 |
| Sphericity | 0.92 | 0.93 | 0.91 | 0.90 | 0.91 |
| Turbidity (FTU) | 56.4 | 46.8 | 60.2 | 62.2 | 51.6 |
| Acid solubility (%) | 1.4 | 1.5 | 1.4 | 1.5 | 1.6 |
| Percentage of damage/86Mpa (%) | 2.1 | 1.5 | 1.9 | 2.2 | 2.0 |
| Percentage of damage/100Mpa (%) | 4.6 | 5.0 | 5.3 | 5.5 | 4.9 |
As can be seen from Table 2, detect according to SY/T5108-2014 standard-required, the volume density of embodiment 1-5 resultant layer high-strength pressure crack proppant is 1.50g/cm
3below, volume density is 2.50g/cm
3below, the percentage of damage under 86Mpa, 103Mpa pressure is respectively 1.5%, 5.0%, and resistance to compression grade can reach 15K.Experimental result shows, layer high-strength pressure crack proppant of the present invention has the advantages such as ultimate compression strength is high, percentage of damage is low, volume density is low, resistance to corrosion is strong, meet exploitation of oil-gas field requirement completely, and volume density is far below industry standard.
Claims (10)
1. double-layer high strength fracturing propping agents, is characterized in that: comprise ceramic core and the silicon nitride ceramics shell being coated on ceramic core surface, the ratio of described ceramic core diameter and silicon nitride ceramics outer casing thickness is 5 ~ 10:1;
Described ceramic core is made primarily of the core raw material of following mass percent: bauxitic clay 40% ~ 50%, shale 40% ~ 50%, coal gangue 0 ~ 10%;
Described silicon nitride ceramics shell is made primarily of the shell material raw material of following mass percent: silicon nitride 60% ~ 70%, bauxitic clay 30% ~ 40%.
2. double-layer high strength fracturing propping agents according to claim 1, is characterized in that: described ceramic core is made primarily of the core raw material of following mass percent: bauxitic clay 45% ~ 50%, shale 40% ~ 45%, coal gangue 5 ~ 10%.
3. double-layer high strength fracturing propping agents according to claim 1 and 2, is characterized in that: in described core raw material, and bauxitic clay used is low bauxitic clay, and in described low bauxitic clay, the mass content of aluminum oxide is not higher than 50%; In described shell material raw material, bauxitic clay used is alumine, and in described alumine, the mass content of aluminum oxide is not less than 70%.
4. a preparation method for double-layer high strength fracturing propping agents as claimed in claim 1, is characterized in that: comprise the following steps:
1) get the bauxitic clay of formula ratio, shale, coal gangue fine powder, be mixed to get core raw material; Get the silicon nitride of formula ratio, bauxitic clay fine powder, be mixed to get shell material raw material, for subsequent use;
2) by step 1) gained core raw material adds binding agent, inner core blank of granulating to obtain;
3) by step 1) gained shell material raw material adds binding agent, with step 2) gained inner core blank is that core is granulated, form coating layer on inner core blank surface, obtain work in-process;
4) get step 3) gained work in-process dry after carry out roasting, cool and get final product.
5. the preparation method of double-layer high strength fracturing propping agents according to claim 4, is characterized in that: step 1) in, fine powder used meets 500 mesh screen residue≤3%.
6. the preparation method of double-layer high strength fracturing propping agents according to claim 4, is characterized in that: described binding agent to be mass concentration be 0.1% ~ 1.0% polyacrylamide solution, cmc soln or polyglycol solution.
7. the preparation method of the double-layer high strength fracturing propping agents according to claim 4 or 6, is characterized in that: step 2) in, the mass ratio of described core raw material and binding agent is 100:8 ~ 10; Step 3) in, the mass ratio of described shell material raw material and binding agent is 100:8 ~ 12.
8. the preparation method of double-layer high strength fracturing propping agents according to claim 4, is characterized in that: step 3) in, obtain work in-process with 35 ~ 65 object sieved through sieve after granulating.
9. the preparation method of double-layer high strength fracturing propping agents according to claim 4, is characterized in that: step 4) in, the temperature of described roasting is 1300 ~ 1400 DEG C, and the time of roasting is not less than 6h.
10. the preparation method of double-layer high strength fracturing propping agents according to claim 4, is characterized in that: step 4) in, obtain finished product with 40 ~ 70 object sieved through sieve after cooling.
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| CN111335863A (en) * | 2020-04-10 | 2020-06-26 | 西南石油大学 | Channel fracturing method for alternately injecting conventional soluble proppant and capsule soluble proppant |
| CN114230345A (en) * | 2021-11-24 | 2022-03-25 | 吉林大学 | High-strength porous silicon carbide ceramic for molten metal filtration and preparation method thereof |
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| WO2023173576A1 (en) * | 2022-03-18 | 2023-09-21 | 河南天祥新材料股份有限公司 | Ceramic tracing proppant |
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Denomination of invention: A double-layer high-strength fracturing proppant and its preparation method Effective date of registration: 20231127 Granted publication date: 20181211 Pledgee: Bank of China Limited Gongyi Branch Pledgor: HENAN TIANXIANG NEW MATERIALS Co.,Ltd. Registration number: Y2023980067758 |