CN110016330B - Proppant and preparation method thereof - Google Patents
Proppant and preparation method thereof Download PDFInfo
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- CN110016330B CN110016330B CN201910217060.1A CN201910217060A CN110016330B CN 110016330 B CN110016330 B CN 110016330B CN 201910217060 A CN201910217060 A CN 201910217060A CN 110016330 B CN110016330 B CN 110016330B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 132
- 239000000843 powder Substances 0.000 claims abstract description 60
- 239000011812 mixed powder Substances 0.000 claims abstract description 44
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 29
- 239000000853 adhesive Substances 0.000 claims abstract description 25
- 230000001070 adhesive effect Effects 0.000 claims abstract description 25
- 238000005469 granulation Methods 0.000 claims abstract description 21
- 230000003179 granulation Effects 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 66
- 239000002245 particle Substances 0.000 claims description 55
- 239000011521 glass Substances 0.000 claims description 39
- 239000004005 microsphere Substances 0.000 claims description 39
- 238000007385 chemical modification Methods 0.000 claims description 23
- 238000009826 distribution Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 239000003607 modifier Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000003213 activating effect Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- -1 diselenide compound Chemical class 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 239000010881 fly ash Substances 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 5
- 229910001570 bauxite Inorganic materials 0.000 claims description 5
- 238000002715 modification method Methods 0.000 claims description 5
- 229920001568 phenolic resin Polymers 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 239000008187 granular material Substances 0.000 abstract description 17
- 238000003756 stirring Methods 0.000 description 54
- 230000000052 comparative effect Effects 0.000 description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000012530 fluid Substances 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 239000011863 silicon-based powder Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- PEJDSPDYWVKRKX-UHFFFAOYSA-N C(C)O.C(C1=CC=C(C=O)C=C1)=O Chemical compound C(C)O.C(C1=CC=C(C=O)C=C1)=O PEJDSPDYWVKRKX-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 238000001994 activation Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 150000003959 diselenides Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a proppant and a preparation method thereof. The apparent density of the proppant is less than 1.00g/cm3Volume density of less than 0.40g/cm3The proppant comprises the following raw material components by taking the total weight of the raw material components of the proppant as 100 percent: chemically modified60-80% of first powder material, 5-18% of chemically modified second powder material, 15-20% of prepolymer of thermosetting resin adhesive and 1-2% of organic solvent. The preparation method of the proppant comprises the following steps: adding thermosetting resin adhesive and organic solvent into the mixed powder material which is chemically modified for many times, and carrying out adhesion granulation; and drying, solidifying, cooling and sieving the granules obtained by bonding and granulating to obtain the proppant. The proppant can be used for propping the upper part of a hydraulic fracture, and is a better proppant for the upper part of the hydraulic fracture.
Description
Technical Field
The invention relates to a proppant and a preparation method thereof, belongs to the technical field of hydraulic fracturing, and particularly relates to a proppant suitable for the upper part of a hydraulic fracture and a preparation method thereof.
Background
Hydraulic fracture reformation is one of the core technologies for the economic and effective development of low-permeability ultra-low permeability and unconventional oil and gas fields. The proppant is a key material for ensuring high flow conductivity of hydraulic fracture, and the efficient filling of the proppant in the fracture is very important for ensuring the fracturing effect. In the fracturing modification construction process, fracturing fluid is injected into an underground reservoir layer under the conditions of high speed and high pressure to crack the reservoir layer, before the reservoir layer cracks are closed, the fracturing fluid with proppant enters the reservoir layer cracks and supports the cracks, oil and gas fluid is discharged through gaps between the proppant layers under the action of the surface pressure, and finally oil and gas exploitation is realized.
At present, the conventional proppants such as quartz sand, ceramsite and the like commonly used in the industry have higher apparent density which is generally 2.6-3.9g/cm3The high-viscosity fracturing fluid is required to be carried and conveyed, the gel breaking of the high-viscosity fracturing fluid is incomplete, and the high polymer in the high-viscosity fracturing fluid is adsorbed on the rock of a reservoir stratum to easily cause the damage to the reservoir stratum. And when the viscosity of the fracturing fluid is low, the conventional high-density proppant is difficult to suspend, so that the conveying is difficult, the proppant is easy to settle in cracks, and the effective supporting area of the cracks is small. In contrast, ultra low density proppants can be as low as 1.0-1.1g/cm due to density3The density of the proppant is basically equal to that of water, the minimum flow speed required by suspension conveying of the ultra-low density proppant is kept one order of magnitude lower than that of the conventional proppant, the proppant can be conveyed only by clean water or slickwater, the conveying and filling efficiency is high, the effective supporting area of the fracture is large, the problems of incomplete gel breaking and damage to the reservoir by high polymer adsorption do not exist in the clean water or slickwater, the damage of fracturing to the reservoir and artificial fractures can be obviously reduced, the adjustment of the flow conductivity of the fractures is facilitated, and the yield of oil gas is further adjusted. However, both conventional proppants and ultra-low density proppants have apparent densities greater than clear water (density of 1.000 g/cm)3) Or slick water (density of 0.960-1.005 g/cm)3) Proppant with apparent density higher than that of clean or slick water tends to settle within a few days after the pump is stopped and before the fracture closes, causing the upper part of the hydraulic fracture to be unsupported. Generally, the fracture height of a hydraulic fracture propped by a propping agent is less than 40% of the fracture height, the vast upper part of the hydraulic fracture cannot realize effective support, and the hydraulic fracture can be gradually closed under the action of rock closing pressure, so that an oil gas leakage channel is closed, and further the yield is reduced.
At present, no apparent density of < 1.00/cm has been found3The report of (1).
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a proppant and a preparation method thereof. The apparent density of the proppant is less than 1.00g/cm3Volume density of less than 0.40g/cm3The hydraulic support can be kept to be completely suspended in clear water or slick water and hydraulic fractures, and can realize the upper support of the hydraulic fractures.
In order to achieve the above object, the present invention provides a proppant, the apparent density of which is less than 1.00g/cm3Volume density of less than 0.40g/cm3The raw material composition of the proppant comprises a prepolymer of a thermosetting resin adhesive, an organic solvent and a chemically modified mixed powder material; wherein
The chemically modified mixed powder material comprises a chemically modified first powder material and a chemically modified second powder material;
the content of the chemically modified first powder material is 60-80%, the content of the chemically modified second powder material is 5-18%, the content of the prepolymer of the thermosetting resin adhesive is 15-20%, and the content of the organic solvent is 1-2%, wherein the total weight of the components of the proppant raw materials is 100%.
In the above proppant, preferably, the apparent density of the first powder material before chemical modification is 0.35 to 0.70g/cm3The particle size distribution range before chemical modification is 5-45 μm; more preferably, the median particle diameter D before chemical modification50And 24 μm.
In the above proppant, preferably, the apparent density of the second powder material before chemical modification is 2.30 to 3.90g/cm3The particle size distribution range before chemical modification is 1-6 μm; median particle diameter D before chemical modification50And was 4 μm.
In the above proppant, preferably, when the first powder material and the second powder material are chemically modified, the modifier used includes a diselenide compound; preferably, the diselenide compound comprises 1, 2-di-n-hexyl diselenide and/or 1, 2-di-n-decyl diselenide.
In the above proppant, preferably, the ratio of the total weight of the modifier to the total weight of the chemically modified mixed powder material is 1:200 to 1: 50; wherein the total weight of the chemically modified mixed powder material is the sum of the weights of the chemically modified first powder material and the chemically modified second powder material.
When inorganic mineral materials (such as kaolin, montmorillonite, attapulgite, hollow glass microspheres, fly ash, silica micropowder and bauxite) are compounded with organic polymer materials, the inorganic mineral materials are difficult to be effectively compounded with the organic polymer materials due to the difference of oleophylic and hydrophilic properties, and a high-performance proppant product is difficult to be prepared. The invention can effectively solve the problems by using the mixed powder material which is chemically modified.
In a preferred scheme of the invention, powder modification is carried out by using a chemical agent comprising a diselenide compound (such as 1, 2-di-n-hexyl diselenide and/or 1, 2-di-n-decyl diselenide), so that lipophilic modification on inorganic mineral materials can be effectively realized, and the structure of the inorganic mineral materials can be protected and higher strength can be kept. When the inorganic mineral material is subjected to oleophylic modification, a commonly used modifying agent such as a silane coupling agent and/or a titanate coupling agent and/or an organic aldehyde compound needs to be modified by using a modifying agent after etching the inorganic mineral material by using strong acid or strong base if the inorganic mineral material is to be effectively modified, but the strong acid or strong base etching can damage the structure of the low-inorganic mineral material and reduce the strength of the low-inorganic mineral material. When the diselenide compound is adopted for modification, the structures of the hollow glass microspheres and the coal ash powder are not obviously damaged, the risk can be effectively avoided, the compressive strength of the proppant is obviously improved, and the proppant with higher strength and better performance is more favorably obtained.
In the above proppant, preferably, the weight ratio of the prepolymer of the thermosetting resin binder to the organic solvent is 8:1 to 15: 1.
In the proppant, preferably, the ratio of the total weight of the prepolymer of the thermosetting resin binder and the organic solvent to the total weight of the chemically modified mixed powder material is 1:3 to 1: 6; wherein the total weight of the chemically modified mixed powder material is the sum of the weights of the chemically modified first powder material and the chemically modified second powder material.
In the above-mentioned proppant, preferably, the prepolymer of the thermosetting resin binder is in a liquid state having a viscosity of 200-3000mPa · s at 25 ℃; more preferably, the prepolymer of the thermosetting resin adhesive comprises one or more of a prepolymer of a thermosetting epoxy resin, a prepolymer of a thermosetting phenolic resin and a prepolymer of a thermosetting polyurethane resin. In the technical scheme provided by the invention, the prepolymer of the thermosetting resin adhesive is preferably cured at the temperature of 160-220 ℃ for 8-20 minutes to obtain a product with a softening point higher than 180 ℃.
In the proppant, preferably, the heat-resistant temperature of the first powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the first powder material before chemical modification is 83-110 MPa;
in the proppant, preferably, the heat-resistant temperature of the second powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the second powder material before chemical modification is not lower than that of the first powder material before chemical modification.
In the proppant, preferably, the chemically modified first powder material comprises chemically modified fly ash and/or chemically modified hollow glass microspheres.
In the above proppant, preferably, the chemically modified second powder material includes chemically modified fine silica powder and/or chemically modified bauxite.
In the above proppant, preferably, the organic solvent includes one or a combination of two or more of methanol, ethanol, and acetone.
In the above proppant, preferably, the particle size of the proppant is 20 to 200 mesh.
The proppant is preferably prepared by the following proppant preparation method.
The invention also provides a preparation method of the proppant, which comprises the following steps:
adding a thermosetting resin adhesive and an organic solvent into the chemically modified mixed powder material, and carrying out adhesive granulation to obtain granules; and drying, solidifying, cooling and sieving the particles to obtain the proppant.
In the above preparation method, preferably, the chemically modified mixed powder material is prepared by a modification method comprising the steps of:
uniformly mixing the first powder material and the second powder material to obtain a mixed powder material; adding a modifier into the mixed powder material, and then activating at a preset temperature and a preset time to obtain a chemically modified mixed powder material (the material is dried in the activation process, so that the obtained chemically modified mixed powder material is a dried mixed powder material).
In the above modification method, preferably, the predetermined temperature is 60 to 120 ℃, more preferably, 60 to 100 ℃, and further preferably, 70 to 90 ℃.
In the above modification method, preferably, the predetermined time of activation is 1 to 6 hours, more preferably, the predetermined time is 1 to 4 hours, and further preferably, the predetermined time is 2 to 3 hours.
In the above modification method, preferably, when the modifier is added to the mixed powder material, the mixed powder material is in a stirring state, the stirring speed is 1000-1500 rpm, and the modifier is added in portions (for example, but not limited to, 10 portions).
In the above preparation method, preferably, when the particles are dried, the drying temperature is 60 to 100 ℃, and the drying time is 10 to 30 minutes; more preferably, the drying is carried out at a temperature of 80-100 ℃ for a time of 20-30 minutes.
In the above preparation method, preferably, the curing temperature is 160-220 ℃, and the curing time is 8-20 minutes; more preferably, the curing temperature is 180-210 ℃, and the curing time is 10-15 minutes.
In the above preparation method, preferably, the addition of the thermosetting resin binder and the organic solvent to the chemically modified mixed powder material is performed by: adding the mixture of the prepolymer of the thermosetting resin binder and the organic solvent into the chemically modified mixed powder material in batches (for example, but not limited to 10 batches), wherein the chemically modified mixed powder material is stirred at a stirring speed of 1200-3600 rpm; more preferably, the chemically modified mixed powder material is stirred at a stirring speed of 1200-1500 rpm.
In the above preparation method, the stirring speed of the adhesive granulation is preferably 1500-.
In the preparation method, the time for the adhesive granulation is preferably 4000-. In the above preparation method, the granulating equipment may be a granulator.
In one embodiment, the method of making the proppant comprises the steps of:
putting the first powder material and the second powder material into a granulator, and uniformly stirring at the speed of 600-;
adding a modifier to the mixed powder material in batches (for example, but not limited to 10 batches), uniformly mixing, and activating at 60-120 ℃ for 1-6 hours to obtain a chemically modified mixed powder material (the material is dried in the activation process, so that the obtained chemically modified mixed powder material is a dried mixed powder material);
putting the chemically modified mixed powder material into a granulator, and uniformly stirring at the speed of 1200-3600 r/min; then mixing the prepolymer of the thermosetting resin adhesive and the organic solvent, adding the mixture into the granulator in batches (such as but not limited to 10 batches), and increasing the stirring speed of the granulator to 3000-6000 rpm for binding and granulating to obtain granules;
and drying, solidifying, cooling and sieving the particles to obtain the proppant.
In the above embodiment, the stirring at 1200-.
In the above embodiment, the stirring speed of the adhesive granulation is preferably 4000-.
In the above embodiments, the resulting proppant has an apparent density of < 1.00g/cm3。
Compared with the prior art, the invention has the following beneficial effects:
(1) the apparent density of the proppant provided by the invention is less than 1.00g/cm3Volume density of less than 0.40g/cm3. The proppant is an ultra-low density proppant, can be kept to be completely suspended in clear water or slick water and hydraulic fractures, can realize the upper support of the hydraulic fractures, avoids the closure of the fractures after the pump is stopped, and provides more flow guide channels for oil gas discharge, thereby increasing the oil gas yield. In a preferred embodiment of the invention, the particle size distribution of the proppant provided by the invention is 0.850-0.075mm (20-200 meshes), which is more beneficial to field application.
(2) The proppant provided by the invention has a long-term working temperature of more than or equal to 135 ℃, and has small deformation under a certain closing pressure, thereby being beneficial to maintaining higher flow conductivity of a proppant filling layer.
(3) The technical scheme provided by the invention has the advantages of simple preparation method, easy operation and strong repeatability, and is suitable for large-scale industrial production.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides a proppant, and the preparation method comprises the following steps:
2000g of fly ash and 500g of silicon micropowder (the apparent density of the fly ash is 0.35-0.60 g/cm) are added into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D50The heat-resistant temperature of 24 mu m is more than or equal to 500 ℃, and the compressive strength is 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the fly ash), and stirring is carried out for 1 minute at the speed of 1200 revolutions per minute;
25.5g of 1, 2-di-n-hexyldiselenide were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-hexyldiselenide, the mixer-granulator was kept under stirring at 1200 rpm) and thereafter stirring was continued at 1200 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
1275g of the mixed powder material after chemical modification is put into a mixing granulator at one time and stirred for 1 minute at the speed of 2500 rpm;
the stirring speed of the mixing granulator is increased to 3600 revolutions per minute, and mixed liquid is added into the mixing granulator in 10 batches, wherein the mixed liquid is formed by mixing 30g of acetone and 300g of prepolymer of thermosetting phenolic resin;
the stirring speed of the mixing granulator is increased to 4000 revolutions per minute, and the mixture is bonded and granulated for 12 minutes to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 30 minutes, solidifying at 190 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 0.82g/cm3The bulk density is 0.38g/cm3。
Example 2
The embodiment provides a proppant, and the preparation method comprises the following steps:
1800g of hollow glass microspheres (the apparent density of the hollow glass microspheres is 0.35-0.60 g/cm)3The particle size distribution range is 5-45 μm, and the median particle size D50Heat resistance temperature of 24 μm is more than or equal to 500 ℃, compressive strength is 83-110MPa), and 400g of silicon powder (apparent density of silicon powder is 2.30-3.90 g/cm)3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 1000 revolutions per minute;
29.6g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (the mixer-granulator was kept under stirring at 1000 rpm during the addition of 1, 2-di-n-decyldiselenium), after which stirring was continued at 1000 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
1200g of the chemically modified mixed powder material is put into a mixing granulator at one time and stirred for 1 minute at the speed of 1800 rpm;
increasing the stirring speed of the mixing granulator to 3600 revolutions per minute, and adding a mixed solution into the mixing granulator in 10 batches, wherein the mixed solution is formed by mixing 26g of ethanol and 260g of prepolymer of thermosetting epoxy resin;
the stirring speed of the mixing granulator is increased to 4500 rpm, and the particles with proper size are obtained after 16 minutes of bonding granulation;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 185 ℃ for 12 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 0.79g/cm3The bulk density is 0.37g/cm3。
Example 3
The embodiment provides a proppant, and the preparation method comprises the following steps:
2200g of hollow glass microspheres (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator3The particle size distribution range is 5-45 μm, and the median particle size D5024 μm, a heat resistance temperature of not less than 500 ℃ and a compressive strength of 83-110MPa, and 400g of bauxite (the apparent density of the bauxite is 2.30-3.90 g/cm)3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 1000 revolutions per minute;
27g of 1, 2-di-n-hexyldiselenide were added to the mixing granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-hexyldiselenide, the mixing granulator was kept under stirring at 1000 rpm) and thereafter stirring was continued at 1000 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
1500g of the chemically modified mixed powder material is put into a mixing granulator at one time and stirred for 1 minute at the speed of 1500 revolutions per minute;
the stirring speed of the mixing granulator is increased to 3600 revolutions per minute, and mixed liquid is added into the mixing granulator in 10 batches, wherein the mixed liquid is formed by mixing 30g of ethanol and 300g of prepolymer of thermosetting phenolic resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 10 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 190 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 0.78g/cm3The bulk density is 0.36g/cm3。
Example 4
The embodiment provides a proppant, and the preparation method comprises the following steps:
1800g of hollow glass microspheres (the apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator35-45 μm in particle size distribution range, 24 μm in median particle size D50, heat resistance temperature not less than 500 deg.C, and compressive strength 83-110MPa, and 400g of silica micropowder (apparent density of silica micropowder is 2.30-3.90g/cm3, particle size distribution range is 1-6 μm, and median particle size D is504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 1200 revolutions per minute;
27.5g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-decyldiselenium, the mixer-granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
adding 2000g of the mixture of the first powder material and the second powder material into a mixing granulator at one time, and stirring at 1800 rpm for 1 minute;
increasing the stirring speed of the mixing granulator to 4000 revolutions per minute, and adding a mixed solution into the mixing granulator in 10 batches, wherein the mixed solution is formed by mixing 40g of methanol and 400g of a prepolymer of thermosetting epoxy resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 10 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 0.75g/cm3Volume density of 0.35g/cm3。
Example 5
The embodiment provides a proppant, and the preparation method comprises the following steps:
2100g of hollow glass microspheres and 200g of fine silica powder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) were put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D5024 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and the mixture is uniformly stirred at the speed of 1500 revolutions per minute;
adding 25.5g of 1, 2-di-n-hexyldiselenide to the mixing granulator in 10 portions in 5 minutes (during the addition of 1, 2-di-n-hexyldiselenide, the mixing granulator is kept stirring at 1500 rpm), and then continuing to stir at 1500 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
1500g of the mixture of the first powder material and the second powder material is put into a mixing granulator at one time, and the mixture is stirred for 1 minute at the speed of 1500 revolutions per minute;
the stirring speed of the mixing granulator is increased to 3600 revolutions per minute, and mixed liquid is added into the mixing granulator in 10 batches, wherein the mixed liquid is formed by mixing 32g of ethanol and 320g of prepolymer of thermosetting phenolic resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 10 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 195 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 0.72g/cm3The bulk density is 0.34g/cm3。
Comparative example 1
The present comparative example provides a proppant, the method of preparation comprising the steps of:
1636g of hollow glass microspheres (apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator3The particle size distribution range is 5-45 μm, and the median particle size D5024 mu m, the heat-resisting temperature is more than or equal to 500 ℃, the compressive strength is 83-110MPa), and 363g of silicon powder (the apparent density of the silicon powder is 2.30-3.90 g/cm)3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and stirring is carried out at the speed of 1800 rpm for 1 minute;
increasing the stirring speed of the mixing granulator to 4000 revolutions per minute, and adding a mixed solution into the mixing granulator in 10 batches, wherein the mixed solution is formed by mixing 40g of methanol and 400g of a prepolymer of thermosetting epoxy resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 10 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this comparative example was an ultra-low density proppant having an apparent density of 0.75g/cm3Volume density of 0.35g/cm3。
Comparative example 2
The present comparative example provides a proppant, the method of preparation comprising the steps of:
1800g of hollow glass microspheres (the apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator3The particle size distribution range is 5-45 μm, and the median particle size D5024 mu m, the heat-resisting temperature is more than or equal to 500 ℃, the compressive strength is 83-110MPa), and 400g of silicon powder (the apparent density of the silicon powder is 2.30-3.90 g/cm)3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 1200 revolutions per minute;
adding 25g of dilute hydrochloric acid with the concentration of 10 percent by mass into a mixing granulator in 10 batches within 5 minutes (in the process of adding the dilute hydrochloric acid, the mixing granulator is kept stirring at the speed of 1200 rpm), then continuing to stir at the speed of 1200 rpm for 1 minute, then adding 30g of gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 50 percent by mass into the granulator in 5 batches within 2 minutes (in the process of adding the gamma-aminopropyltriethoxysilane aqueous solution, the mixing granulator is kept stirring at the speed of 1200 rpm), then adding 20g of terephthalaldehyde ethanol solution with the concentration of 50 percent by mass into the granulator in 5 batches within 2 minutes (in the process of adding the terephthalaldehyde ethanol solution, the mixing granulator is kept stirring at the speed of 1200 rpm), and then continuing to stir at the speed of 1200 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
adding 2000g of the mixture of the first powder material and the second powder material into a mixing granulator at one time, and stirring at 1800 rpm for 1 minute;
increasing the stirring speed of the mixing granulator to 4000 revolutions per minute, and adding a mixed solution into the mixing granulator in 10 batches, wherein the mixed solution is formed by mixing 40g of methanol and 400g of a prepolymer of thermosetting epoxy resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 10 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this comparative example was a proppant having an apparent density of 1.55g/cm3Volume density of 0.98g/cm3。
Comparative example 3
The comparative example provides a hollow glass microsphere modified with potassium hydroxide and gamma-aminopropyltriethoxysilane, the method of preparation comprising the steps of:
2200g of hollow glass microspheres (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator3The particle size distribution range is 5-45 μm, and the median particle size D5024 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is 83-110MPa) is stirred for 1 minute at the speed of 1200 revolutions per minute;
adding 25g of dilute hydrochloric acid with the concentration of 10 percent by mass into a mixing granulator in 10 batches within 5 minutes (in the process of adding the dilute hydrochloric acid, the mixing granulator is kept stirring at the speed of 1200 rpm), then continuing to stir at the speed of 1200 rpm for 1 minute, then adding 30g of gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 50 percent by mass into the granulator in 5 batches within 2 minutes (in the process of adding the gamma-aminopropyltriethoxysilane aqueous solution, the mixing granulator is kept stirring at the speed of 1200 rpm), then adding 20g of terephthalaldehyde ethanol solution with the concentration of 50 percent by mass into the granulator in 5 batches within 2 minutes (in the process of adding the terephthalaldehyde ethanol solution, the mixing granulator is kept stirring at the speed of 1200 rpm), and then continuing to stir at the speed of 1200 rpm for 1 minute; the material in the mixing granulator was taken out and put into an oven, activated and dried at 80 ℃ for 2 hours.
When the modified hollow glass microspheres are observed under a microscope of 40 times, about 50% of the hollow glass microspheres are broken.
The comparative example also provides a hollow glass microsphere modified by 1, 2-di-n-decyl diselenide, and the preparation method comprises the following steps:
2100g of hollow glass microspheres (apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) were put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, the heat-resisting temperature is more than or equal to 500 ℃, and the compressive strength is 83-110MPa), and the mixture is uniformly stirred at the speed of 1200 r/min;
49.3g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-decyldiselenium, the mixer-granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; the material in the mixing granulator was taken out and put into an oven, activated and dried at 85 ℃ for 2.5 hours.
The modified hollow glass microsphere is observed under a microscope of 40 times, and the breaking proportion of the hollow glass microsphere is less than 5 percent and is far lower than the breaking proportion of the hollow glass microsphere modified by potassium hydroxide and gamma-aminopropyltriethoxysilane in the modification process provided by the comparative example.
Therefore, the strength of the hollow glass microspheres is reduced by modifying the hollow glass microspheres by potassium hydroxide and gamma-aminopropyltriethoxysilane, and if the hollow glass microspheres modified by potassium hydroxide and gamma-aminopropyltriethoxysilane are used as the raw materials of the proppant, the compression resistance of the proppant is not facilitated. In addition, if the hollow glass microspheres modified by potassium hydroxide and gamma-aminopropyltriethoxysilane are used as the raw material of the proppant, the density of the proppant is increased due to the breakage of the hollow glass microspheres, which is one of the reasons why the density of the proppant in comparative example 2 is much higher than that of the proppant provided in examples 1 to 5.
TABLE 1
The proppant products provided in examples 1-5 and comparative examples 1-2 above were subjected to performance tests, the results of which are shown in table 1.
The test of roundness/sphericity and breakage rate is referred to the fracturing propping agent and performance index and test recommendation method in accordance with the oil and gas industry standard SY/T5108-2006 of the people's republic of China.
For the laying concentration is 0.98g/cm2The procedure for testing the compressive deformation amount of the proppant pack at 35MPa and 52MPa is as follows:
weighing a certain weight of proppant by using a balance with an induction quantity of 0.01g, and putting the proppant into a crushing room (the diameter is 50.8mm) recommended by SY/T5108-2006 fracturing proppant and performance index and test recommendation method, so that the filling concentration of the proppant is 0.98g/cm2The initial height of the filling layer is 14.38mm, a piston is placed and rotated by 180 degrees, and the crushing chamber containing the sample is placed on the table surface of a press; and (3) uniformly applying a preset load (35MPa or 52MPa) to the pressurized crushing chamber for 120s at a constant loading time of 60 s. The pressure head of the press has the functions of load control and test and displacement control and test, wherein the load control and measurement precision is 0.01MPa, and the displacement control and measurement precision is 0.01 mm; and when the load is 0.70MPa, the displacement indication of the pressure head is automatically cleared, namely, the deformation quantity counting is started from the moment when the load reaches 0.7MPa, and when the load is stabilized for 120s, the displacement indication of the pressure head is the deformation quantity of the proppant filling layer. The instrument used in the test process is a press (model number is DYZ-300) produced by Jinan general electromechanical technology Limited.
As can be seen from the results in Table 1, the apparent densities of the proppants provided in examples 1-5 and comparative example 1 were each < 1.00g/cm3The volume density is less than 0.40g/cm3All can be suspended in clear water or slick water. However, the proppant provided in examples 1-5 has a significantly better roundness/sphericity than the proppant provided in comparative example 1, and the proppant provided in examples 1-5 has a significantly lower fracture rate and proppant pack deformation amount than the proppant provided in comparative example 1. The hydraulic fracture conductivity with proppant propping is the permeability (K) at the reservoir closure pressuref) And fracture support width: (Wf) It can be seen that, under the condition that the density of the proppant is close and the packing concentration is consistent, the smaller the deformation amount of the proppant packing layer is, the larger the fracture propping gap width is, the higher the fracture conductivity is, and therefore, the proppant provided in examples 1 to 5 is beneficial to maintaining the higher fracture conductivity.
As can be seen from the results in table 1, the proppant provided in comparative example 1, in which the first powder material and the second powder material are not modified, has a plurality of properties significantly lower than those of the proppants provided in examples 1 to 5, which are not favorable for maintaining the upper part of the hydraulic fracture in an open state, maintaining the drainage channel of the oil gas, and increasing the oil gas yield.
As can be seen from table 1 and comparative example 3, the proppant provided in comparative example 2 has a fracture in its structure due to modification of hollow glass microspheres with hydrochloric acid, gamma-aminopropyltriethoxysilane, and terephthalaldehyde during its preparation, resulting in a much higher fracture rate and a much higher amount of filler deformation than those provided in examples 1 to 5 modified with diselenide compounds.
TABLE 2
In addition, the proppants provided in examples 1 to 5 were placed in an oven at 135 ℃ and heated for 30 days, and then were subjected to the fracture rate and compression deformation amount tests again, and the results are shown in table 2. The results in table 2 show that the proppants provided in examples 1-5 still maintain good performance indexes after long-term high-temperature damage.
Claims (23)
1. A proppant, said proppant having an apparent density of less than 1.00g/cm3Volume density of less than 0.40g/cm3The raw material composition of the proppant comprises a prepolymer of a thermosetting resin adhesive, an organic solvent and a chemically modified mixed powder material; wherein,
the chemically modified mixed powder material comprises a chemically modified first powder material and a chemically modified second powder material;
by taking the total weight of the raw materials of the proppant as 100%, the content of the chemically modified first powder material is 60-80%, the content of the chemically modified second powder material is 5-18%, the content of the prepolymer of the thermosetting resin adhesive is 15-20%, and the content of the organic solvent is 1-2%;
wherein the chemically modified first powder material comprises chemically modified fly ash and/or chemically modified hollow glass microspheres; the chemically modified second powder material comprises chemically modified silicon micropowder and/or chemically modified bauxite; when the first powder material and the second powder material are chemically modified, the used modifier comprises 1, 2-di-n-hexyl diselenide and/or 1, 2-di-n-decyl diselenide;
the apparent density of the first powder material before chemical modification is 0.35-0.70g/cm3The particle size distribution range before chemical modification is 5-45 μm;
the apparent density of the second powder material before chemical modification is 2.30-3.90g/cm3The particle size distribution range before chemical modification is 1-6 μm;
the prepolymer of the thermosetting resin adhesive comprises one or the combination of more than two of a prepolymer of thermosetting epoxy resin, a prepolymer of thermosetting phenolic resin and a prepolymer of thermosetting polyurethane resin.
2. The proppant of claim 1, wherein the first powder material has a median particle diameter D prior to chemical modification50And 24 μm.
3. The proppant of claim 1, wherein the second powder material has a median particle diameter D prior to chemical modification50And was 4 μm.
4. The proppant of claim 1,
when the first powder material and the second powder material are chemically modified, the used modifier comprises a diselenide compound;
when the first powder material and the second powder material are chemically modified, the weight ratio of the modifier to the mixed powder material is 1:200-1: 50.
5. The proppant of claim 1,
the weight ratio of the prepolymer of the thermosetting resin adhesive to the organic solvent is 8:1-15: 1;
the ratio of the total weight of the prepolymer of the thermosetting resin adhesive and the organic solvent to the total weight of the chemically modified mixed powder material is 1:3-1: 6.
6. A proppant as set forth in claim 1 wherein said prepolymer of said thermosetting resin binder is in the form of a liquid having a viscosity of 200-3000 mPa-s at 25 ℃.
7. The proppant of claim 1,
the heat-resistant temperature of the first powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the first powder material before chemical modification is 83-110 MPa;
the heat-resistant temperature of the second powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the second powder material before chemical modification is not lower than that of the first powder material before chemical modification.
8. A proppant according to claim 1 wherein said organic solvent comprises one or a combination of two or more of methanol, ethanol and acetone.
9. The proppant of claim 1, wherein the particle size of the proppant is from 20 to 200 mesh.
10. A method of making the proppant of any of claims 1-9, comprising the steps of:
adding a thermosetting resin adhesive and an organic solvent into the chemically modified mixed powder material, and carrying out adhesion granulation to obtain particles;
and drying, solidifying, cooling and sieving the particles to obtain the proppant.
11. The preparation method according to claim 10, wherein the chemically modified mixed powder material is prepared by a modification method comprising the steps of:
uniformly mixing the first powder material and the second powder material to obtain a mixed powder material; and adding a modifier into the mixed powder material, and then activating at a preset temperature and a preset time to obtain the chemically modified mixed powder material.
12. The preparation method according to claim 11, wherein the predetermined temperature at which the modifier is added to the mixed powder material and then activated at the predetermined temperature and the predetermined time is 60 to 120 ℃.
13. The preparation method according to claim 12, wherein the predetermined temperature at which the modifier is added to the mixed powder material and then activated at the predetermined temperature and the predetermined time is 60 to 100 ℃.
14. The preparation method according to claim 13, wherein the predetermined temperature at which the modifier is added to the mixed powder material and then activated at the predetermined temperature and the predetermined time is 70 to 90 ℃.
15. The preparation method according to claim 11, wherein the mixed powder material is added with a modifier and then activated at a predetermined temperature for a predetermined time period of 1 to 6 hours.
16. The preparation method according to claim 15, wherein the mixed powder material is added with a modifier and then activated at a predetermined temperature for a predetermined time for 1 to 4 hours.
17. The preparation method according to claim 16, wherein the mixed powder material is added with a modifier and then activated at a predetermined temperature for a predetermined time of 2 to 3 hours.
18. The method according to claim 10, wherein the drying is carried out at a temperature of 60 to 100 ℃ for 10 to 30 minutes.
19. The method according to claim 18, wherein the drying is carried out at a temperature of 80 to 100 ℃ for 20 to 30 minutes.
20. The method as claimed in claim 10, wherein the curing temperature is 150 ℃ to 200 ℃ and the curing time is 5 to 30 minutes.
21. The method as claimed in claim 20, wherein the curing temperature is 180-200 ℃ and the curing time is 5-15 minutes.
22. The method of claim 10, wherein the time for the adhesive granulation is 5 to 20 minutes.
23. The method of claim 22, wherein the time for the adhesive granulation is 10-15 minutes.
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