CN117142872A - Ceramsite propping agent prepared from high-siliceous raw materials and preparation method thereof - Google Patents
Ceramsite propping agent prepared from high-siliceous raw materials and preparation method thereof Download PDFInfo
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- 239000002994 raw material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000003595 mist Substances 0.000 claims abstract description 5
- 229910001570 bauxite Inorganic materials 0.000 claims description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000006004 Quartz sand Substances 0.000 claims description 29
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- 239000000654 additive Substances 0.000 claims description 19
- 239000005995 Aluminium silicate Substances 0.000 claims description 16
- 230000000996 additive effect Effects 0.000 claims description 16
- 235000012211 aluminium silicate Nutrition 0.000 claims description 16
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 16
- 239000012798 spherical particle Substances 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000012216 screening Methods 0.000 abstract description 4
- 238000005096 rolling process Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- 239000000203 mixture Substances 0.000 description 13
- 238000004321 preservation Methods 0.000 description 13
- 239000012071 phase Substances 0.000 description 8
- 238000010304 firing Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000009703 powder rolling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000010586 diagram Methods 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
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- -1 shale Chemical compound 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- 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
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a ceramsite proppant prepared from high-siliceous raw materials and a preparation method thereof, and relates to the technical field of proppants. Firstly, crushing the raw materials to 1-3mm through a jaw crusher and a twin-roll crusher; grinding to less than 22 μm by a wet ball mill; powder is mixed by a planetary ball mill according to a formula; and (3) putting the mixed raw materials into a granulator for granulating, intermittently adding mist water drops and powder while rolling the powder in the granulator, and finally forming a semi-finished ceramic green body, and screening, drying, sintering and screening the green body to prepare the ceramic proppant. The ceramic proppant prepared by the invention has reasonable proportion, simple process, excellent compressive strength and lower volume density, and can reduce the raw material cost of the ceramic proppant and improve the output of oil and gas fields.
Description
Technical Field
The invention relates to the technical field of propping agents, in particular to a ceramsite propping agent prepared from high-siliceous raw materials and a preparation method thereof.
Background
Propping agents are indispensable materials in oil and gas resource exploitation, are pumped into a stratum along with fracturing fluid in hydraulic fracturing work, play roles in preventing fracture closure, increasing the flow guiding rate and increasing the oil and gas resource yield, and can be divided into three types according to materials: quartz sand, a coated propping agent and a ceramsite propping agent. The quartz sand is taken from the nature, has the advantages of low cost, easy obtainment and the like, but is only suitable for shallow reservoirs due to relatively low compressive strength. The high-strength polymer material is coated on the surface of the quartz sand to improve the compressive strength of the coated propping agent, and the coated propping agent has oleophylic and hydrophobic effects according to the similar principle of molecules, is particularly suitable for exploitation of special stratum, but has higher preparation cost. In contrast, the ceramsite propping agent has higher strength, lower cost and good chemical stability, and can more easily support cracks, increase the flow-guiding rate and realize the aim of increasing the yield.
Ceramsite supportThe agent is a typical fracturing propping agent. The main raw material of the traditional ceramic proppant is high-grade bauxite (Al 2 O 3 Along with the gradual shortage of high-grade bauxite resources, the preparation cost of the ceramsite propping agent is obviously increased, and the propping agent prepared by taking the high-grade bauxite as a raw material generally has higher volume density and apparent density, so that the propping agent is precipitated in the fracturing operation process and is not beneficial to playing a role in diversion. The middle-low grade bauxite accounts for 70 percent of the total bauxite, and Al in the low grade bauxite 2 O 3 The content can reach 40-60%, and the ceramic proppant is an ideal raw material for preparing ceramic propping agents through optimizing components and formulas, besides, cobblestones, quartz sand, shale, kaolin and other high-siliceous raw materials are used as widely existing natural resources in China, and are used as remainder and waste materials in many industrial production, so that the ceramic propping agents with high-siliceous raw materials and low-grade bauxite are developed, and the ceramic propping agents are excellent ways for solving the problem of high production cost of the ceramic propping agents.
In order to solve the problems, a most commonly used means at present is to add a proper amount of sintering aid, and CN 102633492A discloses a production process for preparing a ceramic proppant by using low-grade bauxite, which is characterized by comprising the following components in percentage by weight: 45-70% Al 2 O 3 、20~50%SiO 2 、1.5~4%TiO 2 Also contains K 2 O、Na 2 O, caO, mgO, where Al 2 O 3 The main material is mainly introduced from low-grade bauxite ore; siO (SiO) 2 Mainly introduced by auxiliary material kaolin and main material low-grade bauxite ore, caO and MgO are mainly introduced by auxiliary material calcium carbonate and talcum and TiO 2 Mainly comprises an auxiliary material of titanium concentrate and a main material of low-grade bauxite ore. CN 111620673a discloses a high-strength low-density ceramsite proppant and a preparation method thereof. The ceramsite propping agent comprises the following components in percentage by mass: 47-60% of low-grade bauxite, 25-40% of porcelain stone, 5-15% of waste products produced by ceramsite propping agents, 0.3-0.5% of industrial boric acid, 3-10% of magnesia clay and 2.5-3.6% of silica fume. How to reduce the production cost of the ceramic proppant while obtaining excellent performance becomes the fieldThe problem to be solved is urgent.
Disclosure of Invention
Object of the invention
The invention aims to provide a ceramsite proppant prepared from high-siliceous raw materials and a preparation method thereof, and aims to provide a method for preparing the ceramsite proppant from cobbles, quartz sand, shale, bauxite, kaolin and additives. The low-density high-strength ceramsite proppant composed of corundum and mullite is prepared by crushing the raw materials to less than 22 mu m and performing the procedures of mixing, granulating, drying, sintering and the like.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: a ceramsite propping agent prepared from high-siliceous raw materials is prepared from the following components in percentage by mass:
high siliceous raw materials: 0-75% of cobble, 0-85% of shale and 0-28% of quartz sand;
high aluminum raw material: bauxite 0-35%, kaolin 0-44%;
additive: self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 0% -5% of composite powder;
wherein the mass percentage of the high aluminum raw material is not less than 15 percent, and the mass percentage of the high siliceous raw material is not less than 56 percent.
The cobblestones, the quartz sand and the shale are used for improving the strength of the ceramsite propping agent; the shale and bauxite are used for reducing sintering temperature and improving strength and compactness; the kaolin, quartz sand and shale are used for adjusting the aluminum-silicon ratio of the raw materials; the composite powder is used for providing crystal nucleus to control the crystal formation.
Further, siO in the cobble 2 The content is 85.41% -90.52%;
SiO in the shale 2 The content is 65.72 to 73.46 percent, al 2 O 3 The content is 13.06% -21.06%;
SiO in the quartz sand 2 The content is 76.31% -83.3%;
SiO in the bauxite 2 The content is 17.32% -22.78%, al 2 O 3 The content is 57.64% -63.10%, tiO 2 The content is 2.59% -3.26%;
SiO in the kaolin 2 The content is 19.43-21.56%, al 2 O 3 The content is 51.62-53.37 percent, fe 2 O 3 The content is 7.34% -7.98%, tiO 2 The content is 2.13-2.28%;
the self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 The SiC content in the composite powder is 62-68%, al 2 O 3 The content is 27% -30%, ga 2 O 3 The content is 5% -8%.
Further, the composite material is prepared from the following components in percentage by mass:
high siliceous raw materials: 30% of cobble, 30% of shale and 13% of quartz sand;
high aluminum raw material: 25% of bauxite;
additive: self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 2% of composite powder.
A method of preparing the ceramsite proppant of claim 1, the method of preparing comprising the steps of:
(1) Crushing the high-siliceous raw materials and the high-alumina raw materials to 1-3mm through a jaw crusher and a twin-roll crusher respectively;
(2) Grinding the material obtained in the step (1) to less than 22 mu m through a wet ball mill;
(3) Weighing the powder obtained in the step (2) and the additive according to the mass percentage, and uniformly mixing the components by a ball mill for standby;
(4) Fully combining the powder obtained in the step (3) with mist water drops through a granulator to prepare spherical particle green bodies with certain strength;
(5) And (3) drying the spherical particle green body obtained in the step (4) for 80-12 h, then placing the green body into a box-type resistance furnace, sintering at a high temperature of 1000-1300 ℃, and cooling to obtain the ceramsite proppant.
Further, the powder obtained in the step (2) has a particle size of 18-21 mu m and a water content of 10-12%.
Further, the particle size of the spherical particle green body in the step (4) is 0.212-0.425mm.
(III) beneficial effects
Compared with the prior art, the invention provides the ceramsite proppant prepared from the high-siliceous raw materials and the preparation method thereof, and the ceramsite proppant has the following beneficial effects:
1. the ceramic proppant prepared from the high-siliceous raw materials and the preparation method thereof adopt cobblestones, quartz sand, shale, bauxite, kaolin and additives, so that the cost is effectively reduced.
2. The invention utilizes the wet ball mill to crush the raw materials to less than 22 mu m, the powder is easier to uniformly mix, and the prepared spherical particles are more compact.
3. The volume density of the ceramic proppant is 1.29-1.41g/cm < 3 >, the breaking rate is less than 9% under the closing pressure of 69MPa, and the ceramic proppant has the advantages of reasonable proportion, simple process, low preparation cost and excellent performance, and is suitable for industrial production.
Drawings
FIG. 1 shows the phase composition of a ceramsite proppant prepared by adding shale with different contents after sintering at 1140 ℃;
fig. 2 shows the phase composition of a ceramsite proppant prepared by adding 15.0. 15.0 wt% quartz sand after sintering at temperature;
FIG. 3 shows the phase composition of a ceramsite proppant prepared by adding different-granularity wet ball-milling cobble raw materials after being sintered at 1140 ℃;
FIG. 4 phase composition of a ceramsite proppant with cobble material added at different sintering temperatures;
FIG. 5 shows the phase composition of sintered ceramsite proppants added with different contents of dry ball-milling cobble raw materials at 1140 ℃;
FIG. 6 examples 15, 16, 17 formulation ceramsite proppant phase composition at different sintering temperatures;
FIG. 7 SEM photograph of acid etching after firing ceramsite proppants with different cobbles added at 1140 ℃;
fig. 8 SEM photographs of acid etching of ceramsite proppants added with 15.0. 15.0 wt% quartz sand after different sintering temperatures;
FIG. 9 is a cross-sectional SEM photograph of a ceramic proppant added with wet ball-milled cobbles of different particle sizes;
FIG. 10 is an SEM photograph of acid etching of a ceramic proppant added with 4.4 μm wet ball-milled cobble after different sintering temperatures;
FIG. 11 is an SEM photograph of acid etching after firing ceramsite proppants with different contents of dry ball-milled cobbles at 1140 ℃;
fig. 12 is an SEM photograph of acid etching after addition of 15.0. 15.0 wt% dry ball milled quartz powder of ceramsite proppant at different sintering temperatures.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments.
Example 1
Weighing the following components in percentage by mass:
46% of cobble, 20% of quartz sand, 32% of bauxite, and additives (self-propagating synthetic SiC/Al) 2 O 3 /Ga 2 O 3 Composite powder) 2%
The preparation of the ceramsite propping agent comprises the following steps:
(1) Crushing the raw materials to 1-3mm through a jaw crusher and a twin-roll crusher respectively;
(2) Grinding to 18-21 μm with wet ball mill, and controlling water content to 10-12%;
(3) Adding the obtained powder and the additive into a ball mill with the rotating speed of 150r/min according to the proportion, and uniformly mixing the powder for later use;
(4) Adding the mixed powder into a granulator, and adding 12-13% of mist water drops and a small amount of powder in the powder rolling process until the powder grows to spherical particle green bodies with the particle size of 0.212-0.425 mm; screening and fishing out the obtained spherical particle green bodies, cleaning a granulator, and then adding the spherical particle green bodies into the granulator again to roll for 30 minutes to obtain smooth and compact ceramic green bodies;
(5) And drying the obtained ceramic green body for 80-12 h, then placing the ceramic green body into a box-type resistance furnace, sintering the ceramic green body under the high-temperature condition of 1190 ℃ heat preservation for 2h, and cooling the ceramic green body to obtain a ceramic proppant finished product.
Example 2
Unlike example 1, the ceramic proppant was prepared and sintered at 1250 ℃ for 2 hours at high temperature.
Example 3
Unlike example 1, the ceramic proppant was prepared and sintered at 1270deg.C for 2h under high temperature conditions.
Example 4
Different from example 1, the following components were weighed in percentage by mass: 48% of cobble, 20% of quartz sand and 32% of kaolin; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1150 ℃ and 2h of heat preservation.
Example 5
Different from example 1, the following components were weighed in percentage by mass: 46% of cobble, 20% of quartz sand, 32% of kaolin and 2% of additive; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of keeping the temperature at 1240 ℃ for 2 hours.
Example 6
Different from example 1, the following components were weighed in percentage by mass: 46% of cobble, 20% of quartz sand, 32% of kaolin and 2% of additive; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1260 ℃ and heat preservation for 2 hours.
Example 7
Different from example 1, the following components were weighed in percentage by mass: shale 55%, quartz sand 28%, bauxite 15% and additive 2%; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of heat preservation at 1230 ℃ for 2 hours.
Example 8
Different from example 1, the following components were weighed in percentage by mass: shale 55%, quartz sand 25%, bauxite 15% and additive 5%; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of heat preservation at 1100 ℃ for 2 hours.
Example 9
Different from example 1, the following components were weighed in percentage by mass: 83% of shale, 15% of bauxite and 2% of additive; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1120 ℃ and 2h of heat preservation.
Example 10
Different from example 1, the following components were weighed in percentage by mass: 57% of shale, 28% of quartz sand and 15% of bauxite; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of heat preservation at 1080 ℃ for 2 hours.
Example 11
Different from example 1, the following components were weighed in percentage by mass: 40% of cobble, 18% of quartz sand, 40% of kaolin and 2% of additive; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of keeping the temperature at 1240 ℃ for 2 hours.
Example 12
Unlike example 11, the ceramic proppant was prepared and sintered at 1220 ℃ for 2 hours at high temperature.
Example 13
Different from example 1, the following components were weighed in percentage by mass: 55% of cobble, 18% of quartz sand, 25% of kaolin and 2% of additive; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1280 ℃ and 2h of heat preservation.
Example 14
Unlike example 13, the ceramic proppant was prepared and sintered at 1260 ℃ for 2 hours at high temperature.
Example 15
Different from example 1, the following components were weighed in percentage by mass: 30% of cobble, 13% of quartz sand, 25% of bauxite, 30% of shale and 2% of additive; when the ceramsite proppant is prepared, sintering is carried out under the high-temperature condition of 1180 ℃ and 2h of heat preservation.
Example 16
Unlike example 15, the ceramic proppant was prepared and sintered at 1160 c under high temperature conditions for 2 hours.
Example 17
Unlike example 15, the ceramic proppant was prepared and sintered at 1140 deg.c for 2h at high temperature.
In the above examples, the contents of the components in the raw materials are:
SiO in cobble 2 The content is 85.41% -90.52%;
SiO in shale 2 The content is 65.72 to 73.46 percent, al 2 O 3 The content is 13.06% -21.06%;
SiO in quartz sand 2 The content is 76.31% -83.3%;
SiO in bauxite 2 The content is 17.32% -22.78%, al 2 O 3 The content is 57.64% -63.10%, tiO 2 The content is 2.59% -3.26%;
SiO in kaolin 2 The content is 19.43-21.56%, al 2 O 3 The content is 51.62-53.37 percent, fe 2 O 3 The content is 7.34% -7.98%, tiO 2 The content is 2.13-2.28%;
self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 The SiC content in the composite powder is 62-68%, al 2 O 3 The content is 27% -30%, ga 2 O 3 The content is 5% -8%.
Through XRD phase analysis of the raw materials, the main raw materials of the ceramsite proppant prepared by the method are SiO 2 、Al 2 O 3 、Fe 2 O 3 、K 2 O、Na 2 O、TiO 2 . Therefore, the following comparative examples, in which low-grade bauxite was used as the main raw material, were used for comparative analysis of product properties, and SiO as the raw material in the following comparative examples 2 The content is mainly prepared from different low-grade bauxite, so that the high-siliceous raw materials are not contained.
Comparative example 1
Weighing the following components in percentage by mass:
82% of high-aluminum low-grade bauxite, 14% of high-iron low-grade bauxite, 2% of high-alkali low-grade bauxite and 2% of high-silicon low-grade bauxite;
the preparation of the ceramsite propping agent comprises the following steps:
(1) Crushing the raw materials to 1-3mm through a jaw crusher and a twin-roll crusher respectively;
(2) Grinding to 18-21 μm with wet ball mill, and controlling water content to 10-12%;
(3) Adding the obtained powder and the additive into a ball mill with the rotating speed of 150r/min according to the proportion, and uniformly mixing the powder for later use;
(4) Adding the mixed powder into a granulator, and adding 12-13% of mist water drops and a small amount of powder in the powder rolling process until the powder grows to spherical particle green bodies with the particle size of 0.212-0.425 mm; screening and fishing out the obtained spherical particle green bodies, cleaning a granulator, and then adding the spherical particle green bodies into the granulator again to roll for 30 minutes to obtain smooth and compact ceramic green bodies;
(5) And drying the obtained ceramic green body for 80-12 h, then placing the ceramic green body into a box-type resistance furnace, sintering the ceramic green body under the high-temperature condition of 1280 ℃ heat preservation for 2h, and cooling the ceramic green body to obtain a ceramic proppant finished product.
Comparative example 2
The components are weighed according to the following mass percentages, which are different from comparative example 1: 84% of high-aluminum low-grade bauxite, 4% of high-iron low-grade bauxite, 10% of high-alkali low-grade bauxite and 2% of high-silicon low-grade bauxite; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1300 ℃ and 2h of heat preservation.
Comparative example 3
The components are weighed according to the following mass percentages, which are different from comparative example 1: 80% of high-aluminum low-grade bauxite, 4% of high-iron low-grade bauxite, 4% of high-alkali low-grade bauxite and 12% of high-silicon low-grade bauxite; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1380 ℃ and 2h of heat preservation.
Comparative example 4
The components are weighed according to the following mass percentages, which are different from comparative example 1: high aluminum type low-grade bauxite 84%, high iron type low-grade bauxite 8% and high alkali type low-grade bauxite 8%; when the ceramic proppant is prepared, sintering is carried out under the high-temperature condition of 1360 ℃ and heat preservation for 2 hours.
TABLE 1 examples 1-4 ceramsite proppant performance parameters
| Content of test | Industry standard | Example 1 | Example 2 | Example 3 | Example 4 |
| Firing temperature (. Degree. C.) | - | 1190 | 1250 | 1270 | 1150 |
| Bulk density (g/cm) 3 ) | ≤1.5 | 1.27 | 1.30 | 1.30 | 1.30 |
| Apparent density (g/cm) 3 ) | ≤2.8 | 2.45 | 2.44 | 2.44 | 2.44 |
| Crushing ratio (%) | ≤8 | 12.2 | 7.2 | 7.5 | 10.8 |
| Roundness of | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
| Sphericity degree | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
TABLE 1 examples 5-8 ceramsite proppant performance parameters
| Content of test | Industry standard | Example 5 | Example 6 | Example 7 | Example 8 |
| Firing temperature (. Degree. C.) | - | 1240 | 1260 | 1230 | 1100 |
| Bulk density (g/cm) 3 ) | ≤1.5 | 1.32 | 1.29 | 1.39 | 1.41 |
| Apparent density (g/cm) 3 ) | ≤2.8 | 2.48 | 2.39 | 2.40 | 2.47 |
| Crushing ratio (%) | ≤8 | 7.0 | 6.7 | 6.2 | 8.4 |
| Roundness of | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
| Sphericity degree | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
TABLE 1 examples 9-12 ceramsite proppant performance parameters
| Content of test | Industry standard | Example 9 | Example 10 | Example 11 | Example 12 |
| Firing temperature (. Degree. C.) | - | 1120 | 1080 | 1240 | 1220 |
| Bulk density (g/cm) 3 ) | ≤1.5 | 1.41 | 1.32 | 1.32 | 1.32 |
| Apparent density (g/cm) 3 ) | ≤2.8 | 2.52 | 2.48 | 2.43 | 2.43 |
| Crushing ratio (%) | ≤8 | 10.2 | 12.7 | 8.5 | 9.4 |
| Roundness of | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
| Sphericity degree | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
TABLE 1 examples 13-17 ceramsite proppant performance parameters
| Content of test | Industry standard | Example 13 | Example 14 | Example 15 | Example 16 | Example 17 |
| Firing temperature (. Degree. C.) | - | 1280 | 1260 | 1180 | 1160 | 1140 |
| Bulk density (g/cm) 3 ) | ≤1.5 | 1.29 | 1.29 | 1.40 | 1.39 | 1.36 |
| Apparent density (g/cm) 3 ) | ≤2.8 | 2.33 | 2.39 | 2.49 | 2.51 | 2.49 |
| Crushing ratio (%) | ≤8 | 8.1 | 8.1 | 6.2 | 4.3 | 7.7 |
| Roundness of | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 | 0.9 |
| Sphericity degree | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 | 0.9 |
TABLE 2 comparative examples 1-4 ceramsite proppant performance parameters
| Content of test | Industry standard | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Firing temperature (. Degree. C.) | - | 1280 | 1300 | 1380 | 1360 |
| Bulk density (g/cm) 3 ) | ≤1.5 | 1.40 | 1.39 | 1.42 | 1.41 |
| Apparent density (g/cm) 3 ) | ≤2.8 | 2.74 | 2.75 | 2.77 | 2.76 |
| Crushing ratio (%) | ≤8 | 8.1 | 7.8 | 6.1 | 5.8 |
| Roundness of | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
| Sphericity degree | ≥0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
As can be seen from the above table, the ceramic proppant prepared in example 16 was sample-checked, and the performance index was: bulk density of 1.39g/cm 3 The breaking rate under the closing pressure of 69MPa is 4.3 percent, which meets the requirements of the oil and gas industry standard SY/T5108-2014 on the performance of the ceramic proppant.
Cobblestones, quartz sand and shale are used for improving the strength of the ceramsite propping agent; shale and bauxite are used for reducing sintering temperature, improving strength and compactness; kaolin, quartz sand and shale are used for adjusting the aluminum-silicon ratio of the raw materials; the composite powder is used for providing crystal nucleus to control the crystal formation.
As is clear from the raw material formulations of comparative examples 1 and 2, the bauxite content is higher than the content required by the present invention, resulting in an increase in the liquid phase content in the ceramsite proppant, thereby resulting in a decrease in bulk density and apparent density, and an increase in the breakage rate; as can be seen from the raw material formulation of comparative example 3, since the siliceous raw material content is higher than the content required in the present invention, bauxite is lower than the content required in the present invention, resulting in higher sintering temperature. The raw material formulation of comparative example 4 shows that the siliceous raw material is lower than the requirement of the invention, which results in a decrease in the amount of liquid phase in the ceramic proppant and a decrease in the breakage rate.
Figures 1-12 are phase composition diagrams and SEM photographs of the effect of different feedstock ratios, particle sizes, calcination temperatures on the mineral composition content of the final proppant during the experimental process to obtain the optimal feedstock ratios, particle sizes, and calcination temperatures in the examples.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (6)
1. A ceramsite propping agent prepared by utilizing high siliceous raw materials is characterized in that:
the composite material is prepared from the following components in percentage by mass:
high siliceous raw materials: 0-75% of cobble, 0-85% of shale and 0-28% of quartz sand;
high aluminum raw material: bauxite 0-35%, kaolin 0-44%;
additive: self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 0% -5% of composite powder;
wherein the mass percentage of the high aluminum raw material is not less than 15 percent, and the mass percentage of the high siliceous raw material is not less than 56 percent.
2. The ceramsite proppant prepared from high siliceous raw materials according to claim 1, wherein the proppant is prepared from the high siliceous raw materials by: siO in the cobble 2 The content is 85.41% -90.52%;
SiO in the shale 2 The content is 65.72 to 73.46 percent, al 2 O 3 The content is 13.06% -21.06%;
SiO in the quartz sand 2 The content is 76.31% -83.3%;
SiO in the bauxite 2 The content is 17.32% -22.78%, al 2 O 3 The content is 57.64% -63.10%, tiO 2 The content is 2.59% -3.26%;
SiO in the kaolin 2 The content is 19.43-21.56%, al 2 O 3 The content is 51.62-53.37 percent, fe 2 O 3 The content is 7.34% -7.98%, tiO 2 The content is 2.13-2.28%;
the self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 The SiC content in the composite powder is 62-68%, al 2 O 3 The content is 27% -30%, ga 2 O 3 The content is 5% -8%.
3. A ceramsite proppant prepared from a highly siliceous material according to claim 2, characterized in that: the composite material is prepared from the following components in percentage by mass:
high siliceous raw materials: 30% of cobble, 30% of shale and 13% of quartz sand;
high aluminum raw material: 25% of bauxite;
additive: self-propagating synthesis of SiC/Al 2 O 3 /Ga 2 O 3 2% of composite powder.
4. A method of preparing the ceramsite proppant of any one of claims 1 or 3, comprising the steps of:
step (1), crushing the high-siliceous raw materials and the high-alumina raw materials to 1-3mm through a jaw crusher and a twin-roll crusher respectively;
step (2), grinding the material obtained in the step (1) to less than 22 mu m through a wet ball mill;
step (3), weighing the powder obtained in the step (2) and the additive according to the mass percentage, and uniformly mixing the components by a ball mill for standby;
step (4), fully combining the powder obtained in the step (3) with mist water drops through a granulator to prepare spherical particle green bodies with certain strength;
and (5) drying the spherical particle green compact obtained in the step (4) for 80-12 h, then placing the spherical particle green compact into a box-type resistance furnace, sintering at a high temperature of 1000-1300 ℃, and cooling to obtain the ceramsite proppant.
5. The method for preparing the ceramic proppant according to claim 4, wherein: the particle size of the powder obtained in the step (2) is 18-21 mu m, and the water content is 10-12%.
6. The method for preparing the ceramic proppant according to claim 4, wherein: the particle size of the spherical particle green body in the step (4) is 0.212-0.425mm.
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