CN116177881B - Ultralow-density ceramsite fracturing propping agent and preparation method thereof - Google Patents
Ultralow-density ceramsite fracturing propping agent and preparation method thereof Download PDFInfo
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- CN116177881B CN116177881B CN202310148551.1A CN202310148551A CN116177881B CN 116177881 B CN116177881 B CN 116177881B CN 202310148551 A CN202310148551 A CN 202310148551A CN 116177881 B CN116177881 B CN 116177881B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 50
- 239000002893 slag Substances 0.000 claims abstract description 50
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000006004 Quartz sand Substances 0.000 claims abstract description 26
- 239000011435 rock Substances 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000008188 pellet Substances 0.000 claims abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims 2
- 229910001570 bauxite Inorganic materials 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000002910 solid waste Substances 0.000 abstract description 6
- 230000009467 reduction Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 46
- 239000003921 oil Substances 0.000 description 27
- 238000000227 grinding Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 238000005553 drilling Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000000280 densification Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000013081 microcrystal Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000003181 co-melting Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000029087 digestion Effects 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
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/108—Forming porous, sintered or foamed beads
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention relates to an ultralow-density ceramsite fracturing propping agent and a preparation method thereof. The preparation method comprises the following steps: calcining the oil-based rock debris dry slag to obtain calcined dry slag; mixing and ball milling the calcined dry slag and quartz sand tailings to obtain a mixture; granulating the mixture into balls by taking water as a medium to obtain green balls; drying the green pellets, and then carrying out gradient heating sintering to obtain sintered cooked pellets; cooling the sintered balls and sieving. According to the preparation method of the ultralow-density ceramic fracturing propping agent, the oil-based rock debris dry slag is directly utilized and used as a raw material, and the ultralow-density ceramic fracturing propping agent is prepared through low-temperature gradient sintering, so that the problem of continuous reduction of bauxite resources is solved, the production cost is reduced, the recycling utilization of oil-based rock debris dry slag and quartz sand tailings is completed, the ultralow-density ceramic fracturing propping agent is prepared, and the high-added-value utilization of solid wastes is realized.
Description
Technical Field
The invention belongs to the field of oil and gas exploitation, and particularly relates to an ultralow-density ceramsite fracturing propping agent and a preparation method thereof.
Background
The raw material of the artificial ceramic proppant commonly used at present is bauxite, wherein the higher the alumina content is, the higher the density is, and the stronger the strength is. However, in recent years, the ceramic industry of China is rapidly developed, the storage amount of high-quality bauxite with high alumina content is rapidly reduced, if bauxite is still used in a large amount in a propping agent, serious unbalance of bauxite resource supply and demand is caused, and bauxite is reducedThe use amount of soil is particularly important; the common bauxite propping agent adopts a sintering method, the sintering temperature is 1300-1600 ℃, and the energy consumption is high; meanwhile, corundum or mullite phase is used as a main source of the strength of the propping agent, so that the volume density of the traditional propping agent is relatively high, and is usually 1.6-1.8 g/cm 3 Further increases in operating costs (e.g., higher requirements for fracturing fluid performance and pumping conditions) may be achieved, and individual proppant products may utilize internally generated pores to reduce density, but this approach may result in less dense proppant and sacrifice proppant strength.
In addition, with the improvement of crude oil exploitation technology in China, the petroleum output is increased, the oil-based rock debris generation amount is also increased, and the dry slag obtained after oil-based rock debris treatment belongs to common solid waste, and has limited application scenes such as cement admixture and the like because of the high content of barium sulfate. At present, the treatment of the oil-based rock debris dry slag at home and abroad is mainly based on low added value utilization of well site paving, cement admixture, brick making raw materials and the like, and belongs to the non-inequality of the oil-based rock debris dry slag adopted for industrial solid waste digestion, and the value of the oil-based rock debris dry slag is not reflected.
Therefore, the technical scheme of the invention is provided based on the above.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an ultralow-density ceramsite fracturing propping agent and a preparation method thereof.
The invention provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Calcining the oil-based rock debris dry slag to obtain calcined dry slag;
(2) Mixing and ball milling the calcined dry slag and quartz sand tailings to obtain a mixture; the quartz sand tailings are the parts which have lower grade and cannot be sold as quartz sand products after the quartz sand tailings are mined, the silicon dioxide content is 60% -80%, and the added effect is to increase the silicon dioxide which is the main component forming microcrystals;
(3) Granulating the mixture into balls by taking water as a medium to obtain green balls;
(4) Drying the green pellets, and sintering: firstly, preserving heat at 1040-1050 ℃ for 30-50 min, then raising the temperature to 1065-1070 ℃ for 30-40 min, and then preserving heat at 1080-1090 ℃ for 60min to obtain sintered cooked balls; in the step, the multi-stage temperature control is critical, and based on the microcrystalline ceramic theory, when the sintering is carried out, the temperature firstly reaches the lowest co-melting point (1040-1050 ℃) along with the rising of the baking temperature, and the melting phenomenon of the low-melting-point substance begins to appear, so that the particle rearrangement and the pore filling are caused due to the high flow mass transfer speed and high liquid phase sintering densification rate; then the liquid phase is uniformly dispersed at the melting temperature (1065-1070 ℃), and the gaps among the glassy particles are obviously reduced; the temperature is continuously increased to the crystallization temperature (1080-1090 ℃), tiny crystals are grown among glass particles after the crystallization temperature is reached, the densification degree of the glass particles is continuously improved, microcrystals grow to form a microcrystal interweaved structure, and the densification degree and the compressive strength of the particle structure are improved.
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent.
(6) And detecting roundness sphericity, pressure intensity, breakage rate, bulk density and acid solubility of the obtained finished product.
It is emphasized that in order to ensure that the performances such as strength and the like meet the indexes, the method extracts the barium sulfate from the oil-based rock debris dry slag before calcination (effectively avoiding the influence of bubbles generated by partial decomposition in the process of calcining the barium sulfate on the strength of the propping agent and simultaneously reducing the influence of the overlarge density of the barium sulfate on the whole density of the propping agent). After removing barium sulfate components with larger specific gravity from oil-based rock debris dry slag (most barium sulfate is separated by adopting gravity separation), the barium sulfate content in the dry slag after gravity separation is less than or equal to 5%, the inventor repeatedly searches and verifies that the subsequent sintering process is most favored when the barium sulfate content is less than or equal to 5%, the content of the gravity separation is more than or equal to 90% and the barium sulfate can be sold, the main component of the residual dry slag is shale, and the true density is 2.2-2.5 g/cm 3 Less than 3.3-3.5 g/cm of bauxite 3 Therefore, the density of the prepared propping agent is smaller than that of the traditional propping agent on the raw materials, and the density of the prepared propping agent is also far smaller than that of the traditional bauxite-based propping agent.
After barium sulfate was extracted, the components and contents of the oil-based cuttings dry slag are shown in table 1.
Table 1 oil-based cuttings dry slag composition and content
| Composition of the components | SiO 2 | Al 2 O 3 | CaO | MgO | Fe 2 O 3 | BaSO 4 |
| Content/% | 45～55 | 7～20 | 20～35 | ＜5 | ＜5 | ＜2 |
In addition, the quartz sand tailings are the parts which are lower in grade and cannot be sold as quartz sand products after the quartz sand tailings are mined, and the silicon dioxide content is 60% -80%. The effect of adding the quartz sand tailings is to increase the main component silica forming crystallites, which serves to increase the strength of the proppant.
Since quartz sand tailings are also industrial waste itself, the inventors have also tried to add other materials such as blast furnace slag and bauxite as a material for supplementing silica, which is mainly considered, and the comparison results are shown in table 2.
Table 2 comparison results
As can be seen from table 2, when no additives were added, the sintering temperature was relatively high and the breakage rate was higher than 10% (it is considered in the art that the smaller the breakage rate, the better the mechanical properties of the proppant, and conversely the worse, and 10% was the critical value) at a determined pressure, the performance was poor; compared with the addition of blast furnace slag and bauxite, after the addition of quartz sand tailings, the sintering temperature is reduced, the crushing rate is further reduced along with the increase of the doping amount under 86MPa, the addition amount is preferably 20-30%, the quartz sand is further added to 40%, and the reduction of the crushing rate is not obvious; the reduction of the breaking rate is not obvious after the blast furnace slag is added, and the breaking rate is always maintained at about 10 percent, even the basic requirement that the breaking rate is less than 9 percent is difficult to reach; the reduction rate can be reduced to a limited extent after bauxite is added, however, the sintering temperature is greatly increased, and the fuel cost is higher. Therefore, the addition of 20 to 30% of quartz sand is the best choice in comprehensive consideration.
Preferably, in the step (1), the calcination temperature is 700 to 850 ℃. Aims to remove volatile substances and carbonates, and the volatile substances and the carbonates are decomposed at the subsequent sintering temperature to generate bubbles which influence indexes such as the strength of the propping agent.
Preferably, in the step (1), the calcination time is 15-30 min.
Preferably, in the step (2), the weight ratio of the calcined dry slag to the quartz sand tailings is 8-7:2-3.
Preferably, in the step (2), the ball milling is performed until the screen residue of 500 meshes is less than 5%.
Preferably, in the step (3), the green pellets have a particle size of 40 to 70 mesh or 70 to 140 mesh.
Preferably, in the step (4), the drying temperature is 105 ℃, and the drying time is 1-3 h.
The invention also provides the ultralow-density ceramsite fracturing propping agent prepared by the preparation method.
Preferably, the ultra-low density ceramsite fracturing propping agent has a crushing rate of less than 3.5% under 69MPa, a crushing rate of less than 7.5% under 86MPa, an acid solubility of less than 7%, a sphericity of more than 0.8 and a volume density of 1.1-1.3 g/cm 3 。
To facilitate an understanding of the present invention, the following concepts are explained.
And (3) a propping agent: in the oil gas exploitation process, the hydraulic fracture crack is filled and supported so that the hydraulic fracture crack is not closed again, the oil gas can be successfully exploited out of the fracture, and the solid particles with a certain roundness and sphericity are used for achieving the purpose of yield increase.
Ultra low density proppants: proppant density less than 1.5g/cm 3 I.e., an ultra low density proppant, the lower the proppant density, the more capable of being suspended in the fracturing fluid, which can be transported to a greater distance in horizontal drilling and therefore is of greater value.
Oil-based cuttings: in the shale gas exploitation drilling construction process, dangerous waste is composed of oil-based drilling fluid and drilling cuttings. The oil-based rock debris dry slag refers to solid phase remained after oil-water components in the oil-based rock debris are removed through harmless treatment, and the oil content of the dry slag of the sintered ceramsite is lower than 1%.
Sphericity, acid solubility: are all indexes specified by the fracturing propping agent product standard, wherein the sphericity is more than 0.7, and the acid solubility is less than 7%.
The beneficial effects of the invention are as follows:
according to the preparation method of the ultralow-density ceramic fracturing propping agent, the oil-based rock debris dry slag is directly utilized and used as a raw material, and the ultralow-density ceramic fracturing propping agent is prepared through low-temperature gradient sintering, so that the problem of continuous reduction of bauxite resources is solved, the production cost is reduced, the recycling utilization of oil-based rock debris dry slag and quartz sand tailings is completed, the ultralow-density ceramic fracturing propping agent is prepared, and the high-added-value utilization of solid wastes is realized.
Specific:
1. oil-based rock debris dry slag and quartz sand tailings are used as raw materials, other materials are not doped, bauxite propping agents are replaced, exploitation of bauxite resources is reduced, and resources are saved. The sludge dry slag and the quartz sand tailing materials are simple in source and belong to solid wastes, so that the comprehensive utilization of solid waste resources is realized.
2. The sintering temperature is 1090 ℃ at most and is far lower than 1300-1600 ℃ of the bauxite ceramsite fracturing propping agent, so that the energy consumption is greatly saved.
3. The density of the obtained fracturing propping agent body is only 1.1-1.3 g/cm 3 Is obviously lower than that of the traditional propping agent by 1.6-1.8 g/cm 3 Is a bulk density of (c).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
Example 1
The embodiment provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Firstly extracting barium sulfate (the content of the barium sulfate is lower than 5%) from oil-based rock debris dry slag, and then calcining for 30min at 700 ℃ to obtain calcined dry slag;
(2) Mixing the calcined dry slag and quartz sand tailings in a ratio of 7:3, and grinding the mixture to 3% of 500-mesh screen residue by a micropulp mill;
(3) Granulating the mixture into balls in a granulator by taking water as a medium to obtain green balls with the granularity of 40-70 meshes;
(4) Drying the green pellets at 105 ℃ for 1h, then sintering in a rotary kiln, firstly preserving heat at 1040 ℃ for 50min, then preserving heat at 1065 ℃ for 40min, and finally preserving heat at 1080 ℃ for 60min;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent. Wherein, the oversized or undersized unqualified products obtained by screening are returned to the mill for fine grinding and reutilization, thus forming closed cycle.
Example 2
The embodiment provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Firstly extracting barium sulfate (the content of the barium sulfate is lower than 5%) from the oil-based rock debris dry slag, and then calcining for 15min at 850 ℃ to obtain calcined dry slag;
(2) Mixing the calcined dry slag and quartz sand tailings in a ratio of 7:3, and grinding the mixture to obtain a 500-mesh screen residue of 4% by a micropulp mill;
(3) Granulating the mixture into balls in a granulator by taking water as a medium to obtain green balls with the granularity of 40-70 meshes;
(4) Drying the green pellets at 105 ℃ for 1h, sintering in a rotary kiln, firstly preserving heat at 1050 ℃ for 30min, then raising the temperature to 1070 ℃ for 30min, and finally raising the temperature to 1090 ℃ for 60min;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent. Wherein, the oversized or undersized unqualified products obtained by screening are returned to the mill for fine grinding and reutilization, thus forming closed cycle.
Example 3
The embodiment provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Firstly extracting barium sulfate (the content of the barium sulfate is lower than 5%) from the oil-based rock debris dry slag, and then calcining for 22min at 780 ℃ to obtain calcined dry slag;
(2) Mixing the calcined dry slag and quartz sand tailings in a ratio of 7:3, and grinding the mixture to 3.5% of 500-mesh screen residue by a micropulp mill;
(3) Granulating the mixture into balls in a granulator by taking water as a medium to obtain green balls with the granularity of 40-70 meshes;
(4) Drying the green pellets at 105 ℃ for 2 hours, sintering in a rotary kiln, firstly preserving heat at 1045 ℃ for 40min, then raising the temperature to 1070 ℃ for 35min, and finally raising the temperature to 1085 ℃ for 60min;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent. Wherein, the oversized or undersized unqualified products obtained by screening are returned to the mill for fine grinding and reutilization, thus forming closed cycle.
Example 4
The embodiment provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Firstly extracting barium sulfate (the content of the barium sulfate is lower than 5%) from oil-based rock debris dry slag, and then calcining for 30min at 700 ℃ to obtain calcined dry slag;
(2) Mixing the calcined dry slag and quartz sand tailings in a ratio of 7:3, and grinding the mixture to 3% of 500-mesh screen residue by a micropulp mill;
(3) Granulating the mixture into balls in a granulator by taking water as a medium to obtain green balls with the granularity of 70-140 meshes;
(4) Drying the green pellets at 105 ℃ for 1h, then sintering in a rotary kiln, firstly preserving heat at 1040 ℃ for 50min, then preserving heat at 1065 ℃ for 40min, and finally preserving heat at 1080 ℃ for 60min;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent. Wherein, the oversized or undersized unqualified products obtained by screening are returned to the mill for fine grinding and reutilization, thus forming closed cycle.
Example 5
The embodiment provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Firstly extracting barium sulfate (the content of the barium sulfate is lower than 5%) from the oil-based rock debris dry slag, and then calcining for 15min at 850 ℃ to obtain calcined dry slag;
(2) Mixing the calcined dry slag and quartz sand tailings in a ratio of 7:3, and grinding the mixture to obtain a 500-mesh screen residue of 4% by a micropulp mill;
(3) Granulating the mixture into balls in a granulator by taking water as a medium to obtain green balls with the granularity of 70-140 meshes;
(4) Drying the green pellets at 105 ℃ for 1h, sintering in a rotary kiln, firstly preserving heat at 1050 ℃ for 30min, then raising the temperature to 1070 ℃ for 30min, and finally raising the temperature to 1090 ℃ for 60min;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent. Wherein, the oversized or undersized unqualified products obtained by screening are returned to the mill for fine grinding and reutilization, thus forming closed cycle.
Example 6
The embodiment provides a preparation method of an ultralow-density ceramsite fracturing propping agent, which comprises the following steps:
(1) Firstly extracting barium sulfate (the content of the barium sulfate is lower than 5%) from the oil-based rock debris dry slag, and then calcining for 22min at 780 ℃ to obtain calcined dry slag;
(2) Mixing the calcined dry slag and quartz sand tailings in a ratio of 7:3, and grinding the mixture to 3.5% of 500-mesh screen residue by a micropulp mill;
(3) Granulating the mixture into balls in a granulator by taking water as a medium to obtain green balls with the granularity of 70-140 meshes;
(4) Drying the green pellets at 105 ℃ for 2 hours, sintering in a rotary kiln, firstly preserving heat at 1045 ℃ for 40min, then raising the temperature to 1070 ℃ for 35min, and finally raising the temperature to 1085 ℃ for 60min;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent. Wherein, the oversized or undersized unqualified products obtained by screening are returned to the mill for fine grinding and reutilization, thus forming closed cycle.
The fracturing proppants obtained in examples 1 to 6 were tested and the results are shown in table 3.
TABLE 3 detection results
As is clear from Table 3, the volume density of the prepared 69MPa and 86MPa propping agent is 1.1-1.3 g/cm under the condition that other indexes meet the requirements after the extraction of the barium sulfate 3 Within the range, belongs to an ultra-low density ceramsite fracturing propping agent.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. The preparation method of the ultra-low density ceramsite fracturing propping agent is characterized by comprising the following steps of:
(1) Calcining the oil-based rock debris dry slag to obtain calcined dry slag; wherein the calcining temperature is 700-850 ℃, and the calcining time is 15-30 min;
(2) Mixing and ball milling the calcined dry slag and quartz sand tailings to obtain a mixture; wherein the weight ratio of the calcined dry slag to the quartz sand tailings is 8-7:2-3; ball milling until the screen residue of 500 meshes is less than 5%;
(3) Granulating the mixture into balls by taking water as a medium to obtain green balls; wherein the particle size of the green pellets is 40-70 meshes or 70-140 meshes;
(4) Drying the green pellets, and sintering: firstly, preserving heat at 1040-1050 ℃ for 30-50 min, then raising the temperature to 1065-1070 ℃ for 30-40 min, and then preserving heat at 1080-1090 ℃ for 60min to obtain sintered cooked balls; wherein the temperature of the drying is 105 ℃, and the drying time is 1-3 hours;
(5) And cooling the sintered cooked spheres, and screening to obtain the ultra-low density ceramsite fracturing propping agent.
2. The ultra-low density ceramsite fracturing propping agent obtained by the preparation method of claim 1.
3. The ultra-low density ceramic granule fracturing propping agent according to claim 2, wherein the ultra-low density ceramic granule fracturing propping agent has a breakage rate of less than 6% under 69MPa, a breakage rate of less than 6.6% under 86MPa, an acid solubility of less than 6.5%, a sphericity of 0.9 or more and a bulk density of 1.1-1.3 g/cm 3 。
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| US20210040379A1 (en) * | 2020-10-22 | 2021-02-11 | Southwest Petroleum University | Method for preparing low-density proppant by taking oil-based mud wastes as raw materials |
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