CN117185775A - Composite ceramsite and production process thereof - Google Patents
Composite ceramsite and production process thereof Download PDFInfo
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- CN117185775A CN117185775A CN202311158414.2A CN202311158414A CN117185775A CN 117185775 A CN117185775 A CN 117185775A CN 202311158414 A CN202311158414 A CN 202311158414A CN 117185775 A CN117185775 A CN 117185775A
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 119
- 239000002699 waste material Substances 0.000 claims abstract description 101
- 229920001971 elastomer Polymers 0.000 claims abstract description 93
- 239000002994 raw material Substances 0.000 claims abstract description 89
- 239000002245 particle Substances 0.000 claims description 61
- 238000005245 sintering Methods 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000005520 cutting process Methods 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229920002379 silicone rubber Polymers 0.000 claims description 11
- 229920001875 Ebonite Polymers 0.000 claims description 10
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 8
- 239000004927 clay Substances 0.000 claims description 8
- 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 claims description 8
- 229910052863 mullite Inorganic materials 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 229910001570 bauxite Inorganic materials 0.000 claims description 5
- 239000010459 dolomite Substances 0.000 claims description 3
- 229910000514 dolomite Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 239000010456 wollastonite Substances 0.000 claims description 3
- 229910052882 wollastonite Inorganic materials 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910052570 clay Inorganic materials 0.000 claims description 2
- 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 2
- 238000000034 method Methods 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 9
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 238000013016 damping Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 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 3
- 239000003245 coal Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- QXJJQWWVWRCVQT-UHFFFAOYSA-K calcium;sodium;phosphate Chemical compound [Na+].[Ca+2].[O-]P([O-])([O-])=O QXJJQWWVWRCVQT-UHFFFAOYSA-K 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a composite ceramsite, which comprises a porous inner core and a hard outer shell, wherein the mass ratio of the porous inner core to the hard outer shell is (0.5-1.5): 1; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste material and a flexible rubber waste material with the mass ratio of (10-20) to (1-10); the hard shell is made of a second ceramic raw material. Meanwhile, the invention also provides a production process of the composite ceramsite.
Description
Technical Field
The invention relates to the field of oil and gas exploitation, in particular to a composite ceramsite and a production process thereof.
Background
When petroleum and natural gas is mined in deep well, the high-closure-pressure low-permeability ore deposit is subjected to fracturing treatment, so that the stratum containing the petroleum and the gas is cracked, and the petroleum and the gas are collected from channels formed by the cracks. The ceramic supporting material enters the stratum along with the high-pressure solution to be filled in the stratum cracks, and plays a role in supporting the cracks not to be closed due to stress release, so that the high diversion capacity is maintained, the oil gas is unblocked, and the yield is increased. Practice proves that the oil well fractured by using the ceramsite propping agent can improve the yield by 30-50%, and the service life of the oil and gas well can be prolonged.
The ceramic proppant is prepared by sintering a plurality of raw materials such as high-quality bauxite and the like, and is a substitute for natural quartz sand, glass spheres, metal spheres and the like. For example: the Chinese patent CN113956864A discloses a low-density high-strength ceramic proppant coated by silicon dioxide and a preparation method thereof, wherein the ceramic proppant is taken as an inner core, and the silicon dioxide is deposited on the surface of the ceramic proppant to form a silicon dioxide coated ceramic proppant structure. But is not limited to. According to the technical scheme disclosed in Chinese patent CN113956864A, a ceramic proppant is taken as a core, carbon dioxide is deposited on the surface of ceramic to form a shell, the core-shell structure is unstable, and meanwhile, tetraethoxysilane is taken as a raw material, so that the cost is too high.
In order to solve the above problems, an ideal technical solution is always sought.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, thereby providing a composite ceramsite and a production process thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a composite ceramsite comprises a porous inner core and a hard outer shell with the mass ratio of (0.5-1.5): 1; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste material and a flexible rubber waste material with the mass ratio of (10-20) to (1-10); the hard shell is made of a second ceramic raw material.
In the oxygen-enriched atmosphere with the flow rate of 50-100 ml/min, the temperature is raised from 25 ℃ to 900 ℃ at the temperature rising rate of 5-10 ℃/min, the weight of the rigid rubber waste is reduced by 40-60%, and the weight of the flexible rubber waste is reduced by 60-90%.
The first ceramic raw material and the second ceramic raw material are one or a combination of more of gangue, potassium feldspar, mullite, dolomite, wollastonite, tuff, quartz, clay, bauxite, kaolin and bauxite.
The Shore A hardness of the hard rubber waste is 60-90, and the Shore A hardness of the flexible rubber waste is 10-50.
The production process of the composite ceramsite comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste;
(2) Pretreating a first ceramic raw material and a second ceramic raw material;
(3) Granulating and sintering the pretreated rigid rubber waste, flexible rubber waste and the first ceramic raw material to obtain a porous inner core;
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering, cooling and screening to obtain the ceramic composite material.
In the step (1), cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
In the step (2), the first ceramic raw material and the second ceramic raw material are respectively crushed and ball-milled to obtain first ceramic particles and second ceramic particles; wherein the first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
Sintering schedule in step (3): heating to 300-900 deg.C under vacuum condition, vacuum sintering for 5-30 min, charging oxygen, continuously sintering for 5-10 min, vacuumizing, continuously heating to 900-1100 deg.C, and sintering for 5-30 min.
In the step (4), the pretreated second ceramic raw material is evenly sprayed on the surface of the porous inner core, sintered at 1300-1400 ℃ for 20-50 s, cooled and screened to obtain the ceramic.
Compared with the prior art, the composite ceramsite provided by the invention has outstanding substantive characteristics and remarkable progress, and particularly, the porous inner core is prepared by adopting the rubber waste and the ceramic raw materials, so that the rubber waste is utilized to form a porous structure, and the reinforced oxide in the rubber is fully utilized; meanwhile, a layer of closed ceramic crust is formed on the surface of the porous inner core, so that the strength of the composite ceramsite is improved.
Detailed Description
The technical scheme of the invention is further described in detail through the following specific embodiments. In the following examples, coal gangue is solid waste discharged during coal mining and coal washing, and the main components are as follows: 60 to 65 percent of SiO2, 316 to 18 percent of Al2O, 12.45 to 14.27 percent of Fe2O3, 0.42 to 2.32 percent of CaO, 1.40 to 2.41 percent of MgO, 2.50 to 4 percent of TiO2, 0.007 to 0.24 percent of P2O5, 1.4 to 3.9 percent of K2O+Na2O and 0.008 to 0.03 percent of V2O 5; the main components of the potassium feldspar are as follows: 60.0 to 68.0 percent of SiO2, 15.0 to 22.0 percent of Al2O3, K2O9.05 to 15.0 percent of Na2O 2.00 to 2.55 percent. The main components of the mullite are as follows: 42-45% of Al2O3, less than or equal to 1.0% of Fe2O3, 49-55% of SiO2 and less than or equal to 4.0% of Na 2O; the main component of dolomite is CaMg (CO 3) 2; the main component of wollastonite is Ca3 [ Si3O9 ]; the main components of tuff are as follows: 72-74% of SiO2, 15-18% of Al2O3, 1.5-2.0% of Na2O, 7.0-9.0% of K2O, less than 0.20% of Fe2O3, less than 0.5% of CaO, less than 0.3% of MgO and less than 2.5% of burning loss; the main component of quartz is SiO2; the main components in clay are as follows: 32% -38% of SiO2 and 342% -50% of Al 2O; the hard silicon rubber waste can be waste materials such as silicon rubber for special printing, ceramic rubber tubes, rubber treads and the like; the flexible rubber waste can be medical equipment/electronic element sealing piece liquid silicone rubber waste and damping silicone rubber waste.
Examples
A composite ceramsite comprises a porous inner core and a hard outer shell, wherein the mass ratio of the porous inner core to the hard outer shell is (0.5-1.5): 1, and the volume ratio of the porous inner core to the hard outer shell is (3-6): 1; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste material and a flexible rubber waste material with the mass ratio of (10-20) to (1-10); the hard shell is made of a second ceramic raw material.
In the oxygen-enriched atmosphere with the flow rate of 50-100 ml/min, the temperature is raised from 25 ℃ to 900 ℃ at the temperature rising rate of 5-10 ℃/min, the weight of the rigid rubber waste is reduced by 40-60%, and the weight of the flexible rubber waste is reduced by 60-90%. Wherein, the oxygen-enriched atmosphere can directly adopt air.
The first ceramic raw material and the second ceramic raw material have the same components, and comprise 13 parts of potassium feldspar, 22 parts of mullite and 65 parts of light burned clay in parts by mass.
The Shore A hardness of the hard rubber waste is 60-90, and the Shore A hardness of the flexible rubber waste is 10-50.
The production process of the composite ceramsite comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste; and cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
(2) Pretreating a first ceramic raw material and a second ceramic raw material; respectively crushing and ball milling the first ceramic raw material and the second ceramic raw material to obtain first ceramic particles and second ceramic particles; wherein the first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
(3) Granulating the pretreated rigid rubber waste, flexible rubber waste and first ceramic raw materials, heating to 300-900 ℃ under vacuum environment, vacuum sintering for 5-30 min, charging oxygen, continuously sintering for 5-10 min, vacuumizing, continuously heating to 900-1100 ℃ and sintering for 5-30 min to obtain a porous inner core;
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering at 1300-1400 ℃ for 20-50 s, cooling and screening to obtain the ceramic composite material.
Example 1
A composite ceramsite, which comprises a porous inner core and a hard outer shell; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste and a flexible rubber waste in a mass ratio of 100:13:5; the raw material of the hard shell is a second ceramic raw material; the mass ratio of the porous inner core to the hard outer shell is 1.2:1.
The production process of the composite ceramsite comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste; and cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
Wherein, the rigid rubber waste adopts rubber tread waste with the Shore hardness of 71, the flexible rubber waste adopts damping silica gel waste with the Shore hardness of 15; in an air atmosphere with the flow rate of 50 ml/min, the thermal gravimetric analysis is carried out by heating from 25 ℃ to 900 ℃ at the heating rate of 10 ℃/min, the weight of the rigid rubber waste is reduced by 57.2%, and the weight of the flexible rubber waste is reduced by 69.5%.
(2) Pretreating a first ceramic raw material and a second ceramic raw material; and respectively crushing and ball milling the first ceramic raw material and the second ceramic raw material to obtain first ceramic particles and second ceramic particles.
The first ceramic raw material and the second ceramic raw material have the same components, and comprise 13 parts of potassium feldspar, 22 parts of mullite and 65 parts of light burned clay in parts by mass. The first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
(3) Granulating the pretreated rigid rubber waste, flexible rubber waste and the first ceramic raw material, wherein the particle size is 70-80 meshes, heating to 500-600 ℃ under vacuum environment, vacuum sintering for 20 min, charging oxygen, continuously sintering for 10 min, vacuumizing, continuously heating to 900-1100 ℃ and sintering for 15 min, thus obtaining the porous inner core with the particle size of 40-50 meshes.
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering at 1300-1400 ℃ for 30 s, cooling and screening to obtain the composite ceramsite with the particle size of 30-50 meshes.
Referring to SY 17125-2019 fracturing propping agent performance indexes and an evaluation test method, performing performance detection on the fracturing propping agent obtained in the embodiment 1, wherein the volume density is 1.65 g/cm < 3 >; apparent density 2.89 g/cm3; the breaking rate was 4.0% at a closing pressure of 86 MPa.
Example 2
A composite ceramsite, which comprises a porous inner core and a hard outer shell; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste and a flexible rubber waste in a mass ratio of 100:15:5; the raw material of the hard shell is a second ceramic raw material; the mass ratio of the porous inner core to the hard outer shell is 1.2:1.
The production process of the composite ceramsite comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste; and cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
Wherein, the rigid rubber waste adopts rubber tread waste with the Shore hardness of 71, the flexible rubber waste adopts damping silica gel waste with the Shore hardness of 15; in an air atmosphere with the flow rate of 50 ml/min, the thermal gravimetric analysis is carried out by heating from 25 ℃ to 900 ℃ at the heating rate of 10 ℃/min, the weight of the rigid rubber waste is reduced by 57.2%, and the weight of the flexible rubber waste is reduced by 69.5%.
(2) Pretreating a first ceramic raw material and a second ceramic raw material; and respectively crushing and ball milling the first ceramic raw material and the second ceramic raw material to obtain first ceramic particles and second ceramic particles.
The first ceramic raw material and the second ceramic raw material have the same components, and comprise 13 parts of potassium feldspar, 22 parts of mullite and 65 parts of light burned clay in parts by mass. The first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
(3) Granulating the pretreated rigid rubber waste, flexible rubber waste and the first ceramic raw material, wherein the particle size is 70-80 meshes, heating to 500-600 ℃ under vacuum environment, vacuum sintering for 5-30 min, charging oxygen, continuously sintering for 10 min, vacuumizing, continuously heating to 900-1100 ℃ and sintering for 20 min, thus obtaining the porous inner core with the particle size of 40-50 meshes.
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering at 1300-1400 ℃ for 40-s, cooling and screening to obtain the composite ceramsite with the particle size of 30-50 meshes.
Referring to SY 17125-2019 fracturing propping agent performance indexes and an evaluation test method, performing performance detection on the fracturing propping agent obtained in the embodiment 2, wherein the volume density is 1.62 g/cm < 3 >; apparent density 2.82 g/cm3; the breaking rate was 4.1% at a closing pressure of 86 MPa.
Example 3
A composite ceramsite, which comprises a porous inner core and a hard outer shell; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste and a flexible rubber waste in a mass ratio of 100:10:5; the raw material of the hard shell is a second ceramic raw material; the mass ratio of the porous inner core to the hard outer shell is 1.2:1.
The production process of the composite ceramsite comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste; and cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
Wherein, the rigid rubber waste adopts rubber tread waste with the Shore hardness of 71, the flexible rubber waste adopts damping silica gel waste with the Shore hardness of 15; in an air atmosphere with the flow rate of 50 ml/min, the thermal gravimetric analysis is carried out by heating from 25 ℃ to 900 ℃ at the heating rate of 10 ℃/min, the weight of the rigid rubber waste is reduced by 57.2%, and the weight of the flexible rubber waste is reduced by 69.5%.
(2) Pretreating a first ceramic raw material and a second ceramic raw material; and respectively crushing and ball milling the first ceramic raw material and the second ceramic raw material to obtain first ceramic particles and second ceramic particles.
The first ceramic raw material and the second ceramic raw material have the same components, and comprise 13 parts of potassium feldspar, 22 parts of mullite and 65 parts of light burned clay in parts by mass. The first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
(3) Granulating the pretreated rigid rubber waste, flexible rubber waste and the first ceramic raw material, wherein the particle size is 70-80 meshes, heating to 500-600 ℃ under vacuum environment, vacuum sintering for 15 min, charging oxygen, continuously sintering for 10 min, vacuumizing, continuously heating to 900-1100 ℃ and sintering for 30 min, thus obtaining the porous inner core with the particle size of 40-50 meshes.
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering at 1300-1400 ℃ for 25s, cooling and screening to obtain the composite ceramsite with the particle size of 30-50 meshes.
Referring to SY 17125-2019 fracturing propping agent performance indexes and an evaluation test method, performing performance detection on the fracturing propping agent obtained in the embodiment 3, wherein the volume density is 1.65 g/cm < 3 >; apparent density 2.93 g/cm3; the breaking rate was 4.0% at a closing pressure of 86 MPa.
Example 4
A composite ceramsite, which comprises a porous inner core and a hard outer shell; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste and a flexible rubber waste in a mass ratio of 100:13:7; the raw material of the hard shell is a second ceramic raw material; the mass ratio of the porous inner core to the hard outer shell is 1.2:1.
The production process of the composite ceramsite comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste; and cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
Wherein, the rigid rubber waste adopts rubber tread waste with the Shore hardness of 71, the flexible rubber waste adopts damping silica gel waste with the Shore hardness of 15; in an air atmosphere with the flow rate of 50 ml/min, the thermal gravimetric analysis is carried out by heating from 25 ℃ to 900 ℃ at the heating rate of 10 ℃/min, the weight of the rigid rubber waste is reduced by 57.2%, and the weight of the flexible rubber waste is reduced by 69.5%.
(2) Pretreating a first ceramic raw material and a second ceramic raw material; and respectively crushing and ball milling the first ceramic raw material and the second ceramic raw material to obtain first ceramic particles and second ceramic particles.
The first ceramic raw material and the second ceramic raw material have the same components, and comprise 13 parts of potassium feldspar, 22 parts of mullite and 65 parts of light burned clay in parts by mass. The first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
(3) Granulating the pretreated rigid rubber waste, flexible rubber waste and the first ceramic raw material, wherein the particle size is 70-80 meshes, heating to 800-900 ℃ under vacuum environment, vacuum sintering for 5 min, charging oxygen, continuously sintering for 10 min, vacuumizing, continuously heating to 900-1100 ℃ and sintering for 15 min, thus obtaining the porous inner core with the particle size of 40-50 meshes.
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering at 1300-1400 ℃ for 30 s, cooling and screening to obtain the composite ceramsite with the particle size of 30-50 meshes.
Referring to SY 17125-2019 fracturing propping agent performance indexes and an evaluation test method, performing performance detection on the fracturing propping agent obtained in the embodiment 4, wherein the volume density is 1.60 g/cm < 3 >; apparent density 2.83 g/cm3; the breaking rate was 4.1% at a closing pressure of 86 MPa.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same; while the invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that: modifications may be made to the specific embodiments of the present invention or equivalents may be substituted for part of the technical features thereof; without departing from the spirit of the invention, it is intended to cover the scope of the invention as claimed.
Claims (9)
1. A composite ceramsite, which is characterized in that: comprises a porous inner core and a hard outer shell with the mass ratio of (0.5-1.5) 1; wherein the raw materials of the porous inner core comprise a first ceramic raw material, a rigid rubber waste material and a flexible rubber waste material with the mass ratio of (10-20) to (1-10); the hard shell is made of a second ceramic raw material.
2. The composite ceramsite according to claim 1, wherein: in the oxygen-enriched atmosphere with the flow rate of 50-100 ml/min, the temperature is raised from 25 ℃ to 900 ℃ at the temperature rising rate of 5-10 ℃/min, the weight of the rigid rubber waste is reduced by 40-60%, and the weight of the flexible rubber waste is reduced by 60-90%.
3. The composite ceramsite according to claim 1 or 2, wherein: the first ceramic raw material and the second ceramic raw material are one or a combination of more of gangue, potassium feldspar, mullite, dolomite, wollastonite, tuff, quartz, clay, bauxite, kaolin and bauxite.
4. The composite ceramsite according to claim 1 or 2, wherein: the Shore A hardness of the hard rubber waste is 60-90, and the Shore A hardness of the flexible rubber waste is 10-50.
5. A process for producing the composite ceramic aggregate according to any one of claims 1 to 4, which comprises the following steps:
(1) Pretreating the rigid rubber waste and the flexible rubber waste;
(2) Pretreating a first ceramic raw material and a second ceramic raw material;
(3) Granulating and sintering the pretreated rigid rubber waste, flexible rubber waste and the first ceramic raw material to obtain a porous inner core;
(4) Uniformly spraying a pretreated second ceramic raw material on the surface of the porous inner core, sintering, cooling and screening to obtain the ceramic composite material.
6. The composite ceramsite according to claim 6, wherein: in the step (1), cleaning, cutting and crushing the hard rubber waste in sequence to obtain silicon rubber particles, and cutting and melting the flexible rubber waste to obtain liquid rubber.
7. The composite ceramsite according to claim 6, wherein: in the step (2), the first ceramic raw material and the second ceramic raw material are respectively crushed and ball-milled to obtain first ceramic particles and second ceramic particles; wherein the first ceramic particles have a particle size of less than 70 μm and the second ceramic particles have a particle size of less than 200 nm.
8. The composite ceramsite according to claim 6, wherein: sintering schedule in step (3): heating to 300-900 deg.C under vacuum condition, vacuum sintering for 5-30 min, charging oxygen, continuously sintering for 5-10 min, vacuumizing, continuously heating to 900-1100 deg.C, and sintering for 5-30 min.
9. The composite ceramsite according to claim 6, wherein: in the step (4), the pretreated second ceramic raw material is evenly sprayed on the surface of the porous inner core, sintered at 1300-1400 ℃ for 20-50 s, cooled and screened to obtain the ceramic.
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