CN105131934B - A kind of double-layer high strength fracturing propping agents and preparation method thereof - Google Patents
A kind of double-layer high strength fracturing propping agents and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000011162 core material Substances 0.000 claims abstract description 119
- 239000002994 raw material Substances 0.000 claims abstract description 80
- 239000000919 ceramic Substances 0.000 claims abstract description 67
- 239000011257 shell material Substances 0.000 claims abstract description 65
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 55
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 52
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 59
- 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 20
- 239000011265 semifinished product Substances 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 11
- 229920002401 polyacrylamide Polymers 0.000 claims description 9
- 239000010695 polyglycol Substances 0.000 claims description 5
- 229920000151 polyglycol Polymers 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000005453 pelletization Methods 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 230000006378 damage Effects 0.000 abstract description 16
- 239000003921 oil Substances 0.000 abstract description 13
- 238000007906 compression Methods 0.000 abstract description 11
- 230000006835 compression Effects 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
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- 239000000243 solution Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000006004 Quartz sand Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000012216 screening Methods 0.000 description 7
- 238000009817 primary granulation Methods 0.000 description 5
- 238000009818 secondary granulation Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910052573 porcelain Inorganic materials 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
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 3
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 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
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
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- 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
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- 230000000977 initiatory effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000010977 jade Substances 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
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000004575 stone 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
Abstract
The invention discloses a kind of double-layer high strength fracturing propping agents and preparation method thereof, belong to oil recovery (gas) auxiliary agent technical field.The fracturing propping agents include ceramic core and the silicon nitride ceramics shell for being coated on ceramic core surface, and the ratio of the ceramic core diameter and silicon nitride ceramics outer casing thickness is 5~10:1；The ceramic core is mainly made of the core material raw material of following mass percent: bauxite 40%~50%, shale 40%~50%, gangue 0~10%；The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 60%~70%, bauxite 30%~40%.Double-layer high strength fracturing propping agents of the invention, have many advantages, such as that compression strength is high, percentage of damage is low, apparent density is low, resistance to corrosion is strong, the percentage of damage < 6% under the conditions of 103Mpa, acid solubility < 2%, the exploitation especially suitable for deep-well and ultradeep well oil gas field.
Description
Technical field
The invention belongs to (gas) auxiliary agent technical fields of recovering the oil, and in particular to a kind of double-layer high strength fracturing propping agents, simultaneously
Further relate to a kind of preparation method of double-layer high strength fracturing propping agents.
Background technique
During petroleum, gas extraction, hydraulic fracturing has become the important means of exploitation.Especially China's stone
The condition of storage of oily natural gas has the characteristics that bury that depth, clossing pressure are high, permeability is low；In oil/gas well deep mining process
In, high clossing pressure deposits of low permeability makes Oil gas-containing rock layer split after frac treatment, and oil gas is from the channel of cracking initiation
Collect, fluid is needed to inject rock base at this time, to be more than the pressure of formation fracture intensity, generates rock stratum around pit shaft
Crack forms the channel with high flow conductivity.It is opened to be able to maintain crack, oil gas product can smoothly be produced to ground,
Petroleum propping agent and high-pressure solution are entered stratum together to be filled in rock crack, distribution of the proppant in crack decides
The flow conductivity in crack, after pressure break is completed, crack can be closed on the proppant of filling, therefore proppant plays branch and cracks
The dual role of crack closure is stitched and prevented, crack can be made to keep high flow conductivity, keep oil gas unimpeded, increases yield.
Currently used fracturing propping agents have the particle etc. of quartz sand, haydite and resin coating.Wherein, the price of quartz sand
Generally the least expensive, relative density is low, and convenient for construction pumping, but the intensity of quartz sand is low, sphericity is poor, percentage of damage is high, to reduce
The flow conductivity in crack, is not particularly well suited for the high deep-well of clossing pressure.Sphericity is changed after quartz sand resin coating
Kind, resistant to breakage ability increases substantially, and flow conductivity is better than quartz sand, but still lower than haydite.It is manufactured using aluminium vanadine as major ingredient
Ceramsite propping agent, sphericity, resistant to breakage ability and flow conductivity are all better than quartz sand, are widely used by deep oil/gas well.But
Be haydite apparent density it is bigger than quartz sand, the performance of pumping conditions and fracturing fluid made higher requirement, increase and apply
Work difficulty；Accumulation is easily caused in fracturing process, it is extremely disadvantageous to water conservancy diversion, to influence later period fuel-displaced effect, while to pump
Send power requirement high, it is big to the abrasion of pipeline.
In contrast, low-density propping agent has preferable voidage, and carrying is easier, and can substantially reduce the viscous of fracturing fluid
Degree reduces the injury to pipeline and pump, it might even be possible to realize clean fracturing, difficulty of construction and cost for oil production is effectively reduced；In addition
Low-density propping agent water conservancy diversion lapse rate is relatively low, the oil recovery effect that can have been generated.Therefore low-density propping agent is developed into branch
Support the direction of agent research.
In the prior art, CN101787270B discloses a kind of low-density ceramic proppant, is with bauxite and gangue
Inner core, using bauxite and mangano-manganic oxide as shell, balling-up sintering to get low-density ceramsite, the diameter of the inner core is 0.2~
0.3mm, the partial size of the ball are 0.6~0.95mm, in the inner core weight ratio of bauxite and gangue be 20~80:80~
20；The weight ratio of bauxite and mangano-manganic oxide is 90~97:10~3 in the shell.Gained ceramsite propping agent has intensity
High, low density feature, but the mixture of mangano-manganic oxide and bauxite is used to form shell, the reduction, strong for density
The increase rate of degree is little, while percentage of damage is high, resistance to corrosion is weak, is not met by high clossing pressure, hypotonic stream reservoir makes
It is required that.
Summary of the invention
The object of the present invention is to provide a kind of double-layer high strength fracturing propping agents, solve existing fracturing propping agents compression strength
Feature low, percentage of damage is high, apparent density is high, resistance to corrosion is weak.
A second object of the present invention is to provide a kind of preparation methods of double-layer high strength fracturing propping agents.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
A kind of double-layer high strength fracturing propping agents, including ceramic core and the silicon nitride ceramics for being coated on ceramic core surface
The ratio of shell, the ceramic core diameter and silicon nitride ceramics outer casing thickness is 5~10:1；
The ceramic core is mainly made of the core material raw material of following mass percent: bauxite 40%~50%, shale
40%~50%, gangue 0~10%；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 60%~
70%, bauxite 30%~40%.
Double-layer high strength fracturing propping agents of the invention, including ceramic core and the silicon nitride for being coated on ceramic core surface
Ceramic shell, ceramic core are mainly made of bauxite, shale and gangue, and density is low；Silicon nitride ceramics shell is mainly by nitrogen
SiClx and bauxite are made, and intensity is high；Gained double-layer high strength fracturing propping agents are high with compression strength, percentage of damage is low, view is close
The advantages that low, resistance to corrosion is strong is spent, percentage of damage < 6%, acid solubility < 2%, especially suitable for depth under the conditions of 103Mpa
The exploitation of well and ultradeep well oil gas field.
The granularity of the double-layer high strength fracturing propping agents is 40~70 mesh.
Preferably, the ceramic core is mainly made of the core material raw material of following mass percent: bauxite 45%~
50%, shale 40%~45%, gangue 5~10%.
In the core material raw material, bauxite used is low bauxite, and the mass content of aluminium oxide is not in the low bauxite
Higher than 50%；In the shell material raw material, bauxite used is alumine, and the mass content of aluminium oxide is not in the alumine
Lower than 70%.Preferably, the mass content of aluminium oxide is 40%~50% in low bauxite；Aluminium oxide in the alumine
Mass content is 70%~80%.
Preferably, the specification requirement of each component raw material used is shown in Table 1.
The specification requirement of 1 each component raw material of table
The silicon nitride is alpha silicon nitride or beta silicon nitride.
Preferably, the ceramic core is made of the core material raw material of binder and following mass percent: bauxite
40%~50%, shale 40%~50%, gangue 0~10%；The silicon nitride ceramics shell is by binder and following matter
The shell material raw material of amount percentage is made: silicon nitride 60%~70%, bauxite 30%~40%.Preparation method includes: powdery
Core material raw material is added binder and pelletizes to obtain inner core blank；Binder is added in the shell material raw material of powdery, secondary by core of inner core blank
Granulation forms clad in inner core billet surface, roasts afterwards to obtain the final product.
The binder be mass concentration be 0.1%~1.0% polyacrylamide solution, cmc soln or
Polyglycol solution.
Double-layer high strength fracturing propping agents of the invention, ceramic core and high-intensitive silicon nitride ceramics including low-density
Shell, it is advantageous that:
1. silicon nitride is a kind of ceramic material of high intensity, with performances such as heatproof, pressure resistance, acid and alkali-resistances, while it is anti-
Compressive Strength is very high, can greatly improve the compression strength of proppant and reduce percentage of damage；The compression strength of product of the present invention can be with
Reach 103MPa, percentage of damage < 6%, especially suitable for oil gas field deep-well and the fracturing work of ultradeep well.
2. each raw material component mechanism of action are as follows: core material raw material uses low bauxite, shale, gangue, in high-temperature calcination
Al in bauxite and shale2O3、SiO2Generate the resistance to compression that there is the rodlike mullite crystalline phase of some strength can be improved proppant
Intensity, meanwhile, the carbon in gangue can generate hole of holding one's breath under high-temperature calcination, significantly reduce the apparent density of proppant.
Case material is done using silicon nitride, utilizes Al in itself high intensity and alumine2O3、SiO2Generate the rigid of higher intensity
Jade mutually improves the compression strength of proppant.The ceramic shell that silicon nitride is formed simultaneously has very strong resistance to acid and alkali, reduces branch
Support the acid solubility of agent.The case material that silicon nitride is formed at high temperature has good surface smoothness and sphericity, can be with
It effectively improves the flow conductivity of proppant and reduces the turbidity of proppant.
3. double-layer high strength fracturing propping agents of the invention detect, 40/70 mesh according to SY/T5108-2014 standard requirements
The bulk density of fracturing propping agents is 1.50g/cm3Hereinafter, apparent density is 2.50g/cm3Hereinafter, under 86Mpa, 103Mpa pressure
Percentage of damage be respectively 1.5%, 5.0%, resistance to compression grade can achieve 15K, fully meet exploitation of oil-gas field requirement, and apparent density
Far below professional standard.Meanwhile fracturing propping agents surface smoothness is good, sphericity is high, flow conductivity is significantly promoted, lower view
Density can be reduced the use in pressing crack construction to guanidine glue, be easier to pump, and pressure break cost can be effectively reduced.
A kind of preparation method of above-mentioned double-layer high strength fracturing propping agents, including the following steps:
1) it takes the bauxite, shale, coal gangue powder of formula ratio to be broken into fine powder, mixes to obtain core material raw material；Take the nitrogen of formula ratio
SiClx, bauxite powder are broken into fine powder, mix to obtain shell material raw material, spare；
2) binder, inner core blank of pelletizing to obtain is added in core material raw material obtained by step 1)；
3) binder is added in shell material raw material obtained by step 1), pelletized using inner core blank obtained by step 2) as core,
Inner core blank surface forms clad, obtains semi-finished product；
4) it is roasted after taking the drying of semi-finished product obtained by step 3), cooling to obtain the final product.
In step 1), fine powder used meets 500 mesh screen residue≤3% (mass percent).The core material raw material or shell material are former
Material the preparation method comprises the following steps: each component raw material is first crushed to 5mm or less (preferably 1~5mm) respectively, then respectively after 5~8h of ball milling,
500 meshes are crossed, until the fineness of powder reaches 500 mesh screen residue≤3% (mass percent)；Afterwards by formula ratio mix to get.
The binder be mass concentration be 0.1%~1.0% polyacrylamide solution, cmc soln or
Polyglycol solution.The binder is the aqueous solution that mass concentration is 0.1%~1.0%.
In step 2), the mass ratio of the core material raw material and binder is 100:8~10；In step 3), the shell material is former
The mass ratio of material and binder is 100:8~12.
In step 3), sieve to obtain semi-finished product with the sieve of 35~65 mesh after granulation.
In step 4), the temperature of the drying is 100~200 DEG C.
In step 4), the temperature of the roasting is 1300~1400 DEG C, and the time of roasting is not less than 6h.Preferably, described
The temperature of roasting is 1350~1400 DEG C, and the time of roasting is 6~8h.
In step 4), sieve to obtain finished product with the sieve of 40~70 mesh after cooling.In general, the sieve of screening semi-finished product is wanted
Mesh size than sieving finished product is big, is primarily due to the contraction of high-temperature roasting lower volume, and moisture loss can also cause volume-diminished；
Such screening mode can guarantee high yield rate.
Binder system is added in the preparation method of double-layer high strength fracturing propping agents of the invention, the core material raw material including powdery
Grain (once pelletizing) obtains inner core blank, and binder is added in the shell material raw material of powdery, is the secondary granulation of core in inner core using inner core blank
Billet surface forms clad, rear to roast；Using the double-deck granulating technique, the ceramic core of low-density and the nitridation of high intensity are obtained
Silicon ceramic shell；During the preparation process, it is easier to control the ratio and performance of inner core and outer layer；Gained double-layer high strength pressure break branch
Agent is supportted, sphericity is high, and high-quality, percentage of damage is low, and compression strength with higher and lower density；Preparation process is brief,
Raw material are taken conveniently, and technological parameter is controllable, are suitable for large-scale industrial production.
Further, double-layer high strength fracturing propping agents and preparation method thereof of the invention, core material raw material use low product
Position bauxite and shale are primary raw material, and the production cost of proppant can be greatly reduced；It is also added into gangue simultaneously, is solved
Comprehensive utilization of resources problem has preferable economic and social benefit.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 1 gained double-layer high strength fracturing propping agents of embodiment；
Fig. 2 is the microstructure sectional view of 1 gained double-layer high strength fracturing propping agents of embodiment.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
Embodiment 1
The double-layer high strength fracturing propping agents of the present embodiment, as shown in Figure 1, including ceramic core 1 and being coated in ceramics
The ratio of the silicon nitride ceramics shell 2 on 1 surface of core, the thickness of the diameter and silicon nitride ceramics shell 2 of the ceramic core 1 is 7:
1；
The ceramic core is mainly made of the core material raw material of following mass percent: low bauxite 45%, shale 45%,
Gangue 10%；The mass content of aluminium oxide is 50% in the low bauxite；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 60%, high alumina
Alumina 40%.The mass content of aluminium oxide is 70% in the alumine；
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, including the following steps:
1) it takes low bauxite, shale, gangue first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling again
Ball milling 8h in machine, until the fineness of powder reaches 500 mesh screen residue≤3%, by formula ratio by gained bauxite, shale, fine powder of gangue
Core material raw material is mixed evenly to obtain, it is spare；
It takes silicon nitride, alumine first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling in ball mill again
Gained silicon nitride, alumine fine powder are mixed evenly by formula ratio until the fineness of powder reaches 500 mesh screen residue≤3% by 8h
Shell material raw material is obtained, it is spare；
2) polyacrylamide solution for being 0.1% using the addition mass concentration of core material raw material obtained by step 1) is as binder
(mass ratio of core material raw material and binder is 100:10) is granulated (primary granulation) on pelletizer, obtains inner core blank；
3) polyacrylamide solution for being 0.1% using the addition mass concentration of shell material raw material obtained by step 1) is as binder
(mass ratio of shell material raw material and binder is 100:11) is granulated (two using inner core blank obtained by step 2) as core on pelletizer
Secondary granulation), clad is formed in inner core billet surface, sieves to obtain semi-finished product using 35~65 mesh screens；
4) it takes semi-finished product obtained by step 3) to dry at 100 DEG C, then is cooled to room temperature after roasting 8h under the conditions of 1360 DEG C,
It is got product using the screening of 40~70 mesh screens.
The microstructure sectional view of double-layer high strength fracturing propping agents obtained by the present embodiment is as shown in Figure 2.Fig. 2 is by gained
Proppant is splitted from centre, the picture observed under the microscope.Figure it is seen that gained double-layer high strength pressure break branch
Supportting agent is subsphaeroidal, sphericity height, epigranular；Double-deck structure as we can see from the figure, the color at edge and internal face
Color is had any different, and display material is different, and centre can also be seen that small stomata, integrally reduces the density of proppant.
Embodiment 2
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, including ceramic core 1 and is coated on pottery
The silicon nitride ceramics shell 2 on 1 surface of porcelain inner core, the ratio of the thickness of the diameter and silicon nitride ceramics shell 2 of the ceramic core 1
For 5:1；
The ceramic core is mainly made of the core material raw material of following mass percent: low bauxite 50%, shale 45%,
Gangue 5%；The mass content of aluminium oxide is 40% in the low bauxite；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 70%, high alumina
Alumina 30%.The mass content of aluminium oxide is 80% in the alumine；
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, including the following steps:
1) it takes low bauxite, shale, gangue first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling again
Ball milling 7h in machine, until the fineness of powder reaches 500 mesh screen residue≤3%, by formula ratio by gained bauxite, shale, fine powder of gangue
Core material raw material is mixed evenly to obtain, it is spare；
It takes silicon nitride, alumine first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling in ball mill again
Gained silicon nitride, alumine fine powder are mixed evenly by formula ratio until the fineness of powder reaches 500 mesh screen residue≤3% by 7h
Shell material raw material is obtained, it is spare；
2) polyacrylamide solution for being 0.1% using the addition mass concentration of core material raw material obtained by step 1) is as binder
(mass ratio of core material raw material and binder is 100:8) is granulated (primary granulation) on pelletizer, obtains inner core blank；
3) polyacrylamide solution for being 0.1% using the addition mass concentration of shell material raw material obtained by step 1) is as binder
(mass ratio of shell material raw material and binder is 100:12) is granulated (two using inner core blank obtained by step 2) as core on pelletizer
Secondary granulation), clad is formed in inner core billet surface, sieves to obtain semi-finished product using 35~65 mesh screens；
4) it takes semi-finished product obtained by step 3) to dry at 120 DEG C, then is cooled to room temperature after roasting 7h under the conditions of 1380 DEG C,
It is got product using the screening of 40~70 mesh screens.
Embodiment 3
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, including ceramic core 1 and is coated on pottery
The silicon nitride ceramics shell 2 on 1 surface of porcelain inner core, the ratio of the thickness of the diameter and silicon nitride ceramics shell 2 of the ceramic core 1
For 10:1；
The ceramic core is mainly made of the core material raw material of following mass percent: low bauxite 47%, shale 43%,
Gangue 10%；The mass content of aluminium oxide is 45% in the low bauxite；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 65%, high alumina
Alumina 35%.The mass content of aluminium oxide is 75% in the alumine；
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, including the following steps:
1) it takes low bauxite, shale, gangue first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling again
Ball milling 6h in machine, until the fineness of powder reaches 500 mesh screen residue≤3%, by formula ratio by gained bauxite, shale, fine powder of gangue
Core material raw material is mixed evenly to obtain, it is spare；
It takes silicon nitride, alumine first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling in ball mill again
Gained silicon nitride, alumine fine powder are mixed evenly by formula ratio until the fineness of powder reaches 500 mesh screen residue≤3% by 6h
Shell material raw material is obtained, it is spare；
2) polyacrylamide solution for being 0.1% using the addition mass concentration of core material raw material obtained by step 1) is as binder
(mass ratio of core material raw material and binder is 100:9) is granulated (primary granulation) on pelletizer, obtains inner core blank；
3) polyacrylamide solution for being 0.1% using the addition mass concentration of shell material raw material obtained by step 1) is as binder
(mass ratio of shell material raw material and binder is 100:10) is granulated (two using inner core blank obtained by step 2) as core on pelletizer
Secondary granulation), clad is formed in inner core billet surface, sieves to obtain semi-finished product using 35~65 mesh screens；
4) it takes semi-finished product obtained by step 3) to dry at 150 DEG C, then is cooled to room temperature after roasting 8h under the conditions of 1360 DEG C,
It is got product using the screening of 40~70 mesh screens.
Embodiment 4
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, including ceramic core 1 and is coated on pottery
The silicon nitride ceramics shell 2 on 1 surface of porcelain inner core, the ratio of the thickness of the diameter and silicon nitride ceramics shell 2 of the ceramic core 1
For 7:1；
The ceramic core is mainly made of the core material raw material of following mass percent: low bauxite 50%, shale 50%；
The mass content of aluminium oxide is 45% in the low bauxite；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 60%, high alumina
Alumina 40%.The mass content of aluminium oxide is 70% in the alumine；
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, including the following steps:
1) it takes low bauxite, shale first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling in ball mill again
Until the fineness of powder reaches 500 mesh screen residue≤3% core is mixed evenly to obtain by formula ratio in gained bauxite, shale fine powder by 6h
Material raw material, it is spare；
It takes silicon nitride, alumine first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling in ball mill again
Gained silicon nitride, alumine fine powder are mixed evenly by formula ratio until the fineness of powder reaches 500 mesh screen residue≤3% by 6h
Shell material raw material is obtained, it is spare；
2) cmc soln for being 1.0% using the addition mass concentration of core material raw material obtained by step 1) is as binder
(mass ratio of core material raw material and binder is 100:8) is granulated (primary granulation) on pelletizer, obtains inner core blank；
3) cmc soln for being 1.0% using the addition mass concentration of shell material raw material obtained by step 1) is as binder
(mass ratio of shell material raw material and binder is 100:10) is granulated (two using inner core blank obtained by step 2) as core on pelletizer
Secondary granulation), clad is formed in inner core billet surface, sieves to obtain semi-finished product using 35~65 mesh screens；
4) it takes semi-finished product obtained by step 3) to dry at 180 DEG C, then is cooled to room temperature after roasting 6h under the conditions of 1400 DEG C,
It is got product using the screening of 40~70 mesh screens.
Embodiment 5
The double-layer high strength fracturing propping agents of the present embodiment, structure is with embodiment 1, including ceramic core 1 and is coated on pottery
The silicon nitride ceramics shell 2 on 1 surface of porcelain inner core, the ratio of the thickness of the diameter and silicon nitride ceramics shell 2 of the ceramic core 1
For 10:1；
The ceramic core is mainly made of the core material raw material of following mass percent: low bauxite 43%, shale 47%,
Gangue 10%；The mass content of aluminium oxide is 50% in the low bauxite；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 70%, high alumina
Alumina 30%.The mass content of aluminium oxide is 80% in the alumine；
The preparation method of the double-layer high strength fracturing propping agents of the present embodiment, including the following steps:
1) it takes low bauxite, shale, gangue first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling again
Ball milling 6h in machine, until the fineness of powder reaches 500 mesh screen residue≤3%, by formula ratio by gained bauxite, shale, fine powder of gangue
Core material raw material is mixed evenly to obtain, it is spare；
It takes silicon nitride, alumine first to distinguish and is crushed to 5mm (through jaw crusher) hereinafter, being placed in ball milling in ball mill again
Gained silicon nitride, alumine fine powder are mixed evenly by formula ratio until the fineness of powder reaches 500 mesh screen residue≤3% by 6h
Shell material raw material is obtained, it is spare；
2) polyglycol solution for being 0.5% using the addition mass concentration of core material raw material obtained by step 1) is as binder (core
The mass ratio of material raw material and binder is 100:10), it is granulated (primary granulation) on pelletizer, obtains inner core blank；
3) polyglycol solution for being 0.5% using the addition mass concentration of shell material raw material obtained by step 1) is as binder (shell
The mass ratio of material raw material and binder is 100:10), (secondary system is granulated on pelletizer using inner core blank obtained by step 2) as core
Grain), clad is formed in inner core billet surface, sieves to obtain semi-finished product using 35~65 mesh screens；
4) it takes semi-finished product obtained by step 3) to dry at 200 DEG C, then is cooled to room temperature after roasting 7h under the conditions of 1380 DEG C,
It is got product using the screening of 40~70 mesh screens.
Experimental example
This experimental example carries out double-layer high strength fracturing propping agents obtained by embodiment 1-5 according to SY/T5108-2014 standard
Performance detection, testing result see the table below 2.
The performance test results of double-layer high strength fracturing propping agents obtained by 2 Examples 1 to 5 of table
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Bulk density (g/cm3) | 1.43 | 1.47 | 1.50 | 1.49 | 1.48 |
| Apparent density (g/cm3) | 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 |
From Table 2, it can be seen that being detected according to SY/T5108-2014 standard requirements, layer high-strength press obtained by embodiment 1-5
The bulk density for splitting proppant is 1.50g/cm3Hereinafter, apparent density is 2.50g/cm3Hereinafter, under 86Mpa, 103Mpa pressure
Percentage of damage is respectively 1.5%, 5.0%, and resistance to compression grade can achieve 15K.The experimental results showed that layer high-strength pressure crack of the invention
Proppant has many advantages, such as that compression strength is high, percentage of damage is low, apparent density is low, resistance to corrosion is strong, fully meets exploitation of oil-gas field
It is required that and apparent density be far below professional standard.
Claims (9)
1. a kind of double-layer high strength fracturing propping agents, it is characterised in that: including ceramic core and be coated on ceramic core surface
The ratio of silicon nitride ceramics shell, the ceramic core diameter and silicon nitride ceramics outer casing thickness is 5~10:1；
The ceramic core is mainly made of the core material raw material of following mass percent: bauxite 40%~50%, shale 40%
~50%, gangue 0~10%；
The silicon nitride ceramics shell is mainly made of the shell material raw material of following mass percent: silicon nitride 60%~70%, aluminium
Alumina 30%~40%；
In the core material raw material, bauxite used is low bauxite, and the mass content of aluminium oxide is not higher than in the low bauxite
50%；In the shell material raw material, bauxite used is alumine, and the mass content of aluminium oxide is not less than in the alumine
70%；
The specification requirement of each component raw material used see the table below:
The specification requirement of each component raw material
2. double-layer high strength fracturing propping agents according to claim 1, it is characterised in that: the ceramic core mainly by with
The core material raw material of lower mass percent is made: bauxite 45%~50%, shale 40%~45%, gangue 5~10%.
3. a kind of preparation method of double-layer high strength fracturing propping agents as described in claim 1, it is characterised in that: including following
Step:
1) bauxite, shale, fine powder of gangue for taking formula ratio mix to obtain core material raw material；Take silicon nitride, the bauxite of formula ratio
Fine powder mixes to obtain shell material raw material, spare；
2) binder, inner core blank of pelletizing to obtain is added in core material raw material obtained by step 1)；
3) binder is added in shell material raw material obtained by step 1), pelletized using inner core blank obtained by step 2) as core, in inner core
Billet surface forms clad, obtains semi-finished product；
4) it is roasted after taking the drying of semi-finished product obtained by step 3), cooling to obtain the final product.
4. the preparation method of double-layer high strength fracturing propping agents according to claim 3, it is characterised in that: in step 1),
Fine powder used meets 500 mesh screen residue≤3%.
5. the preparation method of double-layer high strength fracturing propping agents according to claim 3, it is characterised in that: the binder
Polyacrylamide solution, cmc soln or the polyglycol solution for being 0.1%~1.0% for mass concentration.
6. the preparation method of double-layer high strength fracturing propping agents according to claim 3 or 5, it is characterised in that: step 2)
In, the mass ratio of the core material raw material and binder is 100:8~10；In step 3), the matter of the shell material raw material and binder
Amount is than being 100:8~12.
7. the preparation method of double-layer high strength fracturing propping agents according to claim 3, it is characterised in that: in step 3),
It sieves to obtain semi-finished product with the sieve of 35~65 mesh after granulation.
8. the preparation method of double-layer high strength fracturing propping agents according to claim 3, it is characterised in that: in step 4),
The temperature of the roasting is 1300~1400 DEG C, and the time of roasting is not less than 6h.
9. the preparation method of double-layer high strength fracturing propping agents according to claim 3, it is characterised in that: in step 4),
It sieves to obtain finished product with the sieve of 40~70 mesh after cooling.
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| CN111154479B (en) * | 2020-01-23 | 2021-05-07 | 中国石油大学(北京) | Shale debris coated proppant and preparation method and application thereof |
| CN111335863B (en) * | 2020-04-10 | 2021-03-12 | 西南石油大学 | Channel fracturing method for alternately injecting conventional soluble proppant and capsule soluble proppant |
| CN114230345B (en) * | 2021-11-24 | 2022-10-04 | 吉林大学 | High-strength porous silicon carbide ceramic for molten metal filtration and preparation method thereof |
| CN114456797A (en) * | 2022-03-18 | 2022-05-10 | 河南天祥新材料股份有限公司 | Ceramic tracing proppant |
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