CN109575906B - Resin film coated polymer composite proppant particles and preparation method and application thereof - Google Patents
Resin film coated polymer composite proppant particles and preparation method and application thereof Download PDFInfo
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- CN109575906B CN109575906B CN201710897128.6A CN201710897128A CN109575906B CN 109575906 B CN109575906 B CN 109575906B CN 201710897128 A CN201710897128 A CN 201710897128A CN 109575906 B CN109575906 B CN 109575906B
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- 229920005989 resin Polymers 0.000 title claims abstract description 159
- 239000011347 resin Substances 0.000 title claims abstract description 159
- 239000002245 particle Substances 0.000 title claims abstract description 153
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title abstract description 23
- 229920000642 polymer Polymers 0.000 title abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims description 66
- 238000002156 mixing Methods 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 35
- 238000005243 fluidization Methods 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 28
- 238000001723 curing Methods 0.000 claims description 26
- 239000003960 organic solvent Substances 0.000 claims description 26
- 239000012530 fluid Substances 0.000 claims description 23
- 239000011812 mixed powder Substances 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 18
- 239000004005 microsphere Substances 0.000 claims description 18
- 239000007921 spray Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 16
- 239000008187 granular material Substances 0.000 claims description 16
- 238000007873 sieving Methods 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 238000005469 granulation Methods 0.000 claims description 14
- 230000003179 granulation Effects 0.000 claims description 14
- 239000005011 phenolic resin Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000007385 chemical modification Methods 0.000 claims description 12
- 239000003822 epoxy resin Substances 0.000 claims description 12
- 229920000647 polyepoxide Polymers 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 7
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical compound N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 claims description 6
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000010881 fly ash Substances 0.000 claims description 5
- 229920005749 polyurethane resin Polymers 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 229910001570 bauxite Inorganic materials 0.000 claims description 4
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 4
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 4
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 3
- PCSMJKASWLYICJ-UHFFFAOYSA-N Succinic aldehyde Chemical compound O=CCCC=O PCSMJKASWLYICJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000010419 fine particle Substances 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 32
- 238000000576 coating method Methods 0.000 description 21
- 239000003795 chemical substances by application Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 15
- 239000000523 sample Substances 0.000 description 13
- 239000003921 oil Substances 0.000 description 11
- 239000006004 Quartz sand Substances 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229920001187 thermosetting polymer Polymers 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 230000003213 activating effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000005007 epoxy-phenolic resin Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229910052621 halloysite Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 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
- 238000010030 laminating Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 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
- C09K8/805—Coated proppants
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
- E21B43/267—Methods for stimulating production by forming crevices or fractures reinforcing fractures by propping
Landscapes
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides resin film coated polymer composite proppant particles, and a preparation method and application thereof, wherein the apparent density of the resin film coated proppant particles is 1.00-1.08 g/cm3(ii) a The proppant to be coated is 20-100 mesh particles having an apparent density of 1.00-1.10 g/cm3The bulk density is 0.40 to 0.50g/m3(ii) a The proppant to be coated comprises first resin and chemically modified powder which are mutually bonded, wherein the chemically modified powder comprises the chemically modified first powder and the chemically modified second powder. The coated proppant particles can obviously reduce the breaking rate of the proppant and the solubility in the earth acid on the premise of keeping the density of the coated proppant particles unchanged before and after film covering, and are beneficial to reducing the generation of fine particles, thereby improving the flow conductivity of hydraulic fractures to be supported in hydraulic fracturing reconstruction and improving the yield of oil gas.
Description
Technical Field
The invention relates to a resin film coated high polymer composite proppant particle and a preparation method and application thereof, in particular to a resin film coated high polymer composite ultralow density proppant particle and a preparation method and application thereof, belonging to the technical field of oil extraction gas-assisted agents in hydraulic fracturing technology.
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 a fracture reformation construction process, a fracturing fluid is injected at high velocity and high pressure into a subterranean reservoir to fracture it. Before reservoir fractures close, fracturing fluid carrying proppant enters the reservoir fractures and supports the fractures, and oil and gas fluid is discharged through gaps between the proppant layers under the action of the formation pressure, so that oil and gas production is finally realized.
The compression strength of the quartz sand is not high, and when the certain closing pressure (generally 35MPa) is exceeded, more than 15% of the quartz sand is crushed, and fine particles are generated to block reservoir cracks and pores. In addition, the solubility of quartz sand in earth acid is generally over 10%. In order to improve the compressive strength and the soil acid dissolution resistance of the quartz sand, the quartz sand can be coated with a resin film, and the current coating methods of the quartz sand mainly comprise two methods:
the first method is an impregnation method in which quartz sand is impregnated in a resin solution and then dried and cured. The production mode has high energy consumption and low production efficiency, and is basically not used any more.
The second method is a thermal coating method, in which quartz sand and powdered resin are heated together under stirring until the resin is molten (200-250 ℃), and then a resin curing agent is added to cure the coated resin film. For example, CN102942334B discloses a method for coating quartz sand by using a hot coating process.
On the other hand, the apparent density of the quartz sand is generally 2.60 to 2.70g/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 to this, the present invention is,the density of the ultra-low density proppant can be as low as 1.0-1.2 g/cm3The density of the fracturing fluid is basically equal to that of water, the minimum flow speed required by suspension conveying of the proppant 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 low-viscosity fracturing fluid, 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 the low-viscosity fracturing fluid, the damage of fracturing to the reservoir and artificial fractures can be obviously reduced, the fracture conductivity can be improved, and the oil gas yield can be further improved.
The thermal coating method is not suitable for coating the polymer composite material ultra-low density proppant, because the polymer material is softened at the temperature of 200-250 ℃, the polymer composite material ultra-low density proppant particles are adhered, even the polymer material in the polymer composite material ultra-low density proppant particles is damaged, so that the polymer material is excessively aged, and the performance indexes of the polymer composite material ultra-low density proppant in all aspects are reduced; moreover, the products produced by the hot coating method are easy to be consolidated into lumps and have unstable quality. Therefore, the polymer composite material ultra-low density proppant needs to be coated at a lower temperature (such as 50-120 ℃), but in the actual operation process, the resin used for coating at a lower temperature (such as 50-120 ℃) cannot be rapidly cured, so that the proppant particles are mutually adhered and agglomerated, or adhered to the inner wall of a fluidized bed, further fluidization cannot be realized, and production cannot be carried out in serious cases.
CN 103275694 a discloses a polymer composite proppant comprising a natural mineral material (fine silica powder, kaolin, diatomaceous earth or halloysite) and a polyolefin, and a method for coating the proppant with a film, and this patent uses an immersion method. The impregnation method mentioned above is not suitable for industrial production due to low production efficiency.
Therefore, there is a need in the art to develop a method suitable for coating ultra-low density proppant and proppant prepared therefrom to facilitate fracturing modification of oil and gas wells.
Disclosure of Invention
In view of the above-mentioned needs, it is an object of the present invention to provide a resin film coated proppant particle that has the advantages of low fracture rate and low solubility in earth acid when applied to fracture reformation.
The invention also aims to provide a preparation method of the resin film coated proppant particles, which is simple in coating method, strong in operability and easy for industrial production.
It is a further object of the present invention to provide the use of the resin film coated proppant particles described above.
In order to achieve the above objects, in one aspect, the present invention provides a resin film-coated proppant particle having an apparent density of 1.00 to 1.10g/cm3(ii) a The proppant to be coated is 20-100 mesh particles having an apparent density of 1.00-1.08 g/cm3The bulk density is 0.40 to 0.50g/m3(ii) a The proppant to be coated comprises a first resin and chemically modified powder which are mutually bonded;
the chemically modified powder comprises a chemically modified first powder and a chemically modified second powder;
the chemically modified first powder is obtained by chemically modifying a first powder material, and the apparent density of the first powder material is 0.35-0.70 g/cm3The particle size distribution range is 10-90 μm, and the median particle size D5048 mu m and 40-110 MPa of compressive strength;
the second powder subjected to chemical modification is obtained by chemically modifying a second powder material, and the apparent density of the second powder material is 2.30-3.90g/cm3The particle size distribution range before chemical modification is 2-13 mu m, and the median particle size D50Is 8 μm;
the mass ratio of the first resin to the chemically modified first powder to the chemically modified second powder is 40-60: 25-38: 15-20;
the chemical modification refers to the treatment of the first powder material or the second powder material by using modifier alkali and dialdehyde.
Preferably, the base comprises sodium hydroxide and/or potassium hydroxide and the dialdehyde comprises glutaraldehyde and/or succinaldehyde. More preferably, the mass ratio of the alkali to the dialdehyde is 1-3: 3 to 1.
The proppant to be coated is an ultra-low density proppant (polymer composite proppant) with apparent density of 1.00-1.08 g/cm3The bulk density is 0.40 to 0.50g/cm3. Experiments show that the chemical modified mixed powder material (the mixed powder material has the temperature resistance and pressure resistance) and the prepolymer of the thermosetting resin adhesive are used for the proppant to be coated, so that the heat resistance of the proppant can be effectively improved, the working temperature is more than or equal to 160 ℃ for a long time (up to 30 days), and the requirements of fracturing clear water or slickwater fracturing construction of a deep high-temperature oil and gas well can be met; the mixed powder material subjected to chemical modification in the proppant is used as a main component, the prepolymer of the thermosetting resin adhesive is used as an auxiliary component, the proppant has small deformation and small breakage rate under the closed pressure of 10-60 MPa, and the proppant is beneficial to maintaining higher flow conductivity of a proppant filling layer. Further experiments of the invention show that the resin film coated proppant particles are also ultra-low density proppant, the breaking rate and the solubility in earth acid can be obviously reduced under 52MPa, the former is reduced from about 15-18% before coating to about 8-9% after coating, and the latter is reduced from about 13-14% before coating to about 4-5% after coating.
In the above particles of the supporting agent to be coated, preferably, the first powder material includes one or more of chemically modified fly ash and hollow glass microspheres; more preferably, the heat-resistant temperature is 500 ℃.
In the above-mentioned particles of the supporting agent to be coated, preferably, the second powder material includes one or more of chemically modified fine silica powder and bauxite; more preferably, the heat-resistant temperature is 500 ℃.
In the above-mentioned particles of the supporting agent to be coated, preferably, the first resin includes one or more of an epoxy resin, a phenol resin, and a urethane resin.
In the above-mentioned proppant particle to be coated, preferably, the proppant to be coated is prepared by the following method:
uniformly mixing the first powder material and the second powder material to obtain a mixed powder material;
adding the modifier into the mixed powder material, and then modifying at a preset temperature and a preset time to obtain a mixed powder of chemically modified first powder and chemically modified second powder;
adding the mixed powder, the prepolymer of the first resin and the first organic solvent into a granulator for binding granulation to obtain granules;
and drying, solidifying, cooling and sieving the obtained granules to obtain the proppant to be coated.
In the above method for preparing the support agent particle to be coated, the ratio of the total weight of the modifier to the weight of the first powder material or the second powder material is preferably (1:200) to (1: 10);
in the above method for preparing the particles of the supporting agent to be coated, preferably, the first organic solvent includes one or more of methanol, ethanol and acetone.
In the above method for preparing the particles of the supporting agent to be coated, the weight ratio of the prepolymer of the first resin to the first organic solvent is preferably 15-20: 1-2.
In the above method for preparing the particles of the supporting agent to be coated, preferably, the predetermined temperature is 60 to 120 ℃. More preferably 60 to 100 ℃ and still more preferably 70 to 90 ℃.
In the above method for preparing the particles of the supporting agent to be coated, preferably, the predetermined time is 1 to 6 hours. More preferably 1 to 4 hours, and still more preferably 2 to 3 hours.
In the above method for preparing the particles of the support agent to be coated, it is preferable that the drying temperature is 60 to 100 ℃ and the drying time is 10 to 30 minutes when the particles are dried. More preferably, the drying temperature is 80-100 ℃ and the drying time is 20-30 minutes when the particles are dried.
In the above method for preparing the support agent particle to be coated, preferably, the prepolymer of the first resin and the first organic solvent are mixed, and added to the mixed powder in batches at a stirring speed of 1200-3600 rpm. Preferably, the prepolymer of the first resin and the first organic solvent are mixed and then added to the mixed powder in batches at a stirring speed of 1200-1500 rpm.
In the above method for preparing the support agent particles to be coated, preferably, the curing temperature is 150 to 200 ℃, and the curing time is 5 to 30 minutes; more preferably, the curing temperature is 180-200 ℃, and the curing time is 5-15 minutes.
In the above method for preparing the support agent particle to be coated, the time for the binding granulation is preferably 5 to 10 minutes, and preferably 8 to 10 minutes.
In one embodiment, the preparation of the proppant to be coated comprises the steps of:
putting the first powder material and the second powder material into a granulator, and uniformly stirring at the speed of 600-1200 rpm to obtain a mixed powder material;
adding a modifier into the mixed powder material, uniformly mixing, and activating and drying at the temperature of 60-120 ℃ for 1-6 hours to obtain a mixed powder of chemically modified first powder and chemically modified second powder;
putting the obtained mixed powder into a granulator, and uniformly stirring at the speed of 1200-3600 r/min; then mixing the prepolymer of the first resin and a first organic solvent, adding the mixture into the granulator in batches, increasing the stirring speed of the granulator to 3000-6000 rpm, and carrying out bonding granulation to obtain particles;
and drying, solidifying, cooling and sieving the particles to obtain the proppant to be coated.
In the above method for preparing the support agent particle to be coated, preferably, the activated and dried mixed powder is put into a granulator and stirred uniformly at a speed of 2500-3000 r/min.
In the above method for preparing the support agent particle to be coated, preferably, the prepolymer of the first resin and the first organic solvent are added to the granulator in batches, and then the stirring speed of the granulator is increased to 4000 to 5000 rpm.
In the proppant particles coated with the resin film, the mass ratio of the resin film to the proppant particles to be coated is preferably 1:50 to 3: 50.
In the above proppant particle coated with a resin film, the material of the resin film is preferably a reactant of a prepolymer of the second resin and a resin curing accelerator.
In the proppant particle coated with the resin film, the mass ratio of the prepolymer of the second resin to the resin curing accelerator is preferably 70-88: 2-5.
In the above resin film-coated proppant particle, preferably, the prepolymer of the second resin includes one or more of a phenol resin prepolymer, an epoxy resin prepolymer, and a polyurethane prepolymer.
In the above resin film-coated proppant particle, preferably, the resin curing accelerator includes one or more of ammonium chloride, n-propylamine, benzenesulfonic acid, 2,4, 6-tris (dimethylaminomethyl) -phenol, and propylene carbonate.
In another aspect, the present invention provides a method for preparing the resin film-coated proppant, comprising the steps of:
and spraying a solution of a second resin prepolymer and a resin curing accelerator dissolved in a second organic solvent onto the surface of the proppant particles to be coated at a temperature below the softening point of the proppant particles to be coated, and then drying, curing and sieving to obtain the resin film-coated proppant particles.
In the above method for preparing resin film coated proppant, preferably, the proppant particles to be coated are first fluidized by fluid using a spray fluidizing device, then the fluid temperature is raised, and a solution of a second resin prepolymer and a resin curing accelerator dissolved in a second organic solvent is sprayed on the surface of the proppant particles to be coated by using pressurized gas; and after spraying, raising the temperature of the fluid to carry out fluidization and solidification, thus obtaining the proppant particles coated by the resin film.
In the above method for preparing a resin film-coated proppant, preferably, when the first resin is one or more of epoxy resin, phenolic resin and polyurethane resin, the fluid temperature is raised to 60 to 100 ℃ (the temperature can be displayed by a probe of a spray fluidization device); the step of increasing the temperature of the fluid for fluidization and solidification is to increase the temperature to 150-180 ℃ (the temperature can be displayed by a probe of spray fluidization equipment) for fluidization and solidification for 2-10 min.
In the above method for preparing a proppant coated with a resin film, preferably, the fluidizing of the proppant particles to be coated with a fluid is carried out by feeding the proppant particles to be coated to the fluidizing and spraying apparatus in a prescribed amount at a time and fluidizing the proppant particles at an air flow rate of 10 to 50L/min.
In the above method for preparing a resin film-coated proppant, preferably, the spraying of the solution of the second resin prepolymer and the resin curing accelerator dissolved in the second organic solvent onto the surface of the proppant particles to be coated with the pressurized gas is performed by spraying the solution of the second resin prepolymer and the resin curing accelerator dissolved in the second organic solvent onto the surface of the proppant particles to be coated with compressed air at a pressure of 0.2 to 0.5 MPa.
In the above method for preparing a resin film-coated proppant, it is preferable that the resin film-coated proppant comprises 70 wt.% to 88 wt.% of the second resin prepolymer, 10 wt.% to 28 wt.% of the second organic solvent, and 2 wt.% to 5 wt.% of the resin curing accelerator, based on the total weight of the solution of the prepolymer of the second resin and the resin curing accelerator dissolved in the second organic solvent.
In the above method for preparing a resin film-coated proppant, preferably, the prepolymer of the second resin includes one or more of a phenolic resin prepolymer, an epoxy resin prepolymer, and a polyurethane prepolymer.
In the above method for preparing a resin film-coated proppant, preferably, the resin curing accelerator includes one or more of ammonium chloride, n-propylamine, benzenesulfonic acid, 2,4, 6-tris (dimethylaminomethyl) -phenol, and propylene carbonate.
In the above method for preparing a proppant coated with a resin film, the second organic solvent preferably includes one or more of ethanol, methanol, and acetone.
In the above method for preparing a proppant coated with a resin film, the mass ratio of the solution of the prepolymer of the second resin dissolved in the second organic solvent and the resin curing accelerator to the proppant particles to be coated is preferably 1 to 4: 45-55.
In another aspect, the present invention provides the use of the resin film coated proppant particle described above as a proppant in hydraulic fracture modification.
According to the resin film coated proppant particles provided by the invention, on the premise of maintaining the density before and after film coating to be basically unchanged, the breaking rate of the proppant and the solubility in earth acid are remarkably reduced, and the generation of fine particles is favorably reduced, so that the flow conductivity of supporting hydraulic fractures in hydraulic fracturing reconstruction is improved, and the oil gas yield is improved.
In summary, the invention mainly provides resin film coated proppant particles, and a preparation method and application thereof, and the proppant particles can significantly reduce the fracture rate of the proppant and the solubility in earth acid on the premise of maintaining the density of the coated proppant particles before and after coating. The processing temperature used by the method is lower than the softening temperature of the high molecular material in the composite material ultra-low density proppant, the composite material ultra-low density proppant cannot be damaged, and the film laminating method is simple, strong in operability and easy for industrial production.
Detailed Description
The technical solution of the present invention is described in detail and completely with reference to the following embodiments, and it should be understood that the embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a proppant, which comprises the following steps:
1500g of fly ash and 1000g 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 time3Particle size distribution range of 10-90 μm, median particle diameter D5048 mu m, the heat-resisting temperature 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 2-13 μm, median particle diameter D508 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 900 revolutions per minute;
adding 200g of sodium hydroxide aqueous solution with the mass percent concentration of 12.5 percent into a mixing granulator in 10 batches within 5 minutes, then continuing to stir for 2 minutes, subsequently adding 50g of glutaraldehyde aqueous solution with the mass percent concentration of 50 percent into a granulator in 5 batches within 2.5 minutes, and then continuing to stir 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 28g of acetone and 280g 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 8 minutes 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 20-100 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 1.07g/cm3The bulk density is 0.49g/cm3。
Example 2
The embodiment provides a preparation method of a proppant, which comprises the following steps:
1200g of hollow glass microspheres and 1000g of hollow glass microspheres are put into a mixing granulator at one timeg of silicon powder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm)3Particle size distribution range of 10-90 μm, median particle diameter D5048 mu m, the heat-resisting temperature 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 2-13 μm, median particle diameter D508 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not less than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 900 revolutions per minute;
adding 176g of potassium hydroxide aqueous solution with the mass percent concentration of 12.5 percent into the mixing granulator in 10 batches within 5 minutes, then continuing to stir for 2 minutes, subsequently adding 88g of succinic aldehyde aqueous solution with the mass percent concentration of 25 percent into the granulator in 5 batches within 2.5 minutes, and then continuing to stir for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials at 90 ℃ for 1.5 hours;
1122g of the chemically modified mixed powder material was put into a mixing granulator at one time, and stirred at 2500 rpm for 1 minute;
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 mixture is bonded and granulated for 8 minutes 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 20-100 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 1.05g/cm3The bulk density is 0.46g/cm3。
Example 3
The embodiment provides a preparation method of a proppant, which comprises the following steps:
1500g of hollow glass microspheres and 1100g of bauxite (apparent density of hollow glass microspheres: 0.35) were charged into a mixing granulator at a time-0.60g/cm3Particle size distribution range of 10-90 μm, median particle diameter D5048 mu m, the heat-resisting temperature is more than or equal to 500 ℃, and the compressive strength is 83-110 MPa; the bauxite has an apparent density of 2.30-3.90g/cm3Particle size distribution range of 2-13 μm, median particle diameter D508 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not less than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 900 revolutions per minute;
adding 208g of sodium hydroxide aqueous solution with the mass percent concentration of 12.5 percent into the mixing granulator in 10 batches within 5 minutes, then continuing to stir for 2 minutes, subsequently adding 52g of glutaraldehyde aqueous solution with the mass percent concentration of 50 percent into the granulator in 5 batches within 2.5 minutes, and then continuing to stir 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 ℃;
1326g 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;
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 carrying out adhesive granulation for 8 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 20-100 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 1.08g/cm3The bulk density is 0.49g/cm3。
Example 4
The embodiment provides a preparation method of a proppant, which comprises the following steps:
putting 1500g of hollow glass microspheres and 700g of silicon micropowder (apparent density of hollow glass microspheres is 0.35-0.60g/cm3, particle size distribution range is 10-90 μm, and median value isParticle diameter D508 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/cm3, the particle size distribution range is 2-13 μm, and the median particle size D508 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;
176g of an aqueous solution of potassium hydroxide having a concentration of 12.5% by mass are added to the mixing granulator in 10 portions within 5 minutes, stirring is continued for 2 minutes, 44g of an aqueous solution of glutaraldehyde having a concentration of 50% by mass are subsequently added to the granulator in 5 portions within 2.5 minutes, and stirring is continued 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.
1122g of the mixture of the first chemically modified powder material and the second chemically modified powder material was put into a mixing granulator at one time, and stirred 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 20g of methanol and 200g of prepolymer of thermosetting epoxy resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 8 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 20-100 meshes.
The proppant provided by the invention is an ultralow-density proppant, and the apparent density of the proppant is 1.03g/cm3The bulk density is 0.42g/cm3。
Example 5
The embodiment provides a preparation method of a proppant, which comprises the following steps:
1500g of hollow glass microspheres and 800g of silicon micropowder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator at one time3Particle size distribution range of 10-90 μm, median particle diameter D5048 mu m, the heat-resisting temperature 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 2-13 μm, median particle diameter D508 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;
184g of aqueous sodium hydroxide solution having a concentration of 12.5% by mass were added to the mixing granulator in 10 portions over a period of 5 minutes, after which stirring was continued for 2 minutes, and subsequently 46g of aqueous glutaraldehyde solution having a concentration of 50% by mass were added to the granulator in 5 portions over a period of 2.5 minutes, after which stirring was continued for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 3 hours at the temperature of 80 ℃;
1173g of the mixture of the first powder material and the second powder material is put into a mixing granulator at one time, and stirred at 1500 rpm for 1 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 24g of acetone and 240g of prepolymer of thermosetting phenolic resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 8 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 20-100 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 1.02g/cm3Bulk density of 0.41g/cm3。
Comparative example 1
The present comparative example provides a method of preparing a proppant comprising the steps of:
750g of hollow glass microspheres and 400g of silicon micropowder (apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) are added into a mixing granulator at one time3Particle size distribution range of 10-90 μm, median particle diameter D5048 mu m, the heat-resisting temperature 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 2-13 μm, median particle diameter D508 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;
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 24g of acetone and 240g of prepolymer of thermosetting phenolic resin;
increasing the stirring speed of the mixing granulator to 5000 r/min, and performing adhesive granulation for 8 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 20-100 meshes.
The proppant provided in this example was an ultra low density proppant having an apparent density of 1.02g/cm3Bulk density of 0.41g/cm3。
TABLE 1
The proppant products provided in examples 1-5 and comparative example 1 above were tested for performance and the results are shown in table 1.
In Table 1, the fracture rate is tested according 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 amount of compressive deformation of the proppant pack at 35MPa and 52MPa can be tested with reference to the test method in US 6330916B1, the main procedure 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/cm2Placing the piston and rotating the piston by 180 degrees, and placing the crushing chamber with the sample on the table surface of the 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 the displacement reading of the pressure head is automatically cleared when the load is 0.70MPa, and the displacement reading of the pressure head when the load is stabilized for 120s is the deformation 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 proppant pack deformation values provided by examples 1-5 are significantly lower than that of one disclosed in US 6330916B1, which has a density of 1.05g/cm3The proppant (in US 6330916B1, the glass transition temperature of the proppant is 145 ℃, the breakage rate of the proppant at 55MPa and 95 ℃ is less than 0.5 percent, and when the filling concentration of the proppant is 0.98g/cm2The amounts of compressive deformation at 35MPa and 52MPa were 5.77mm and 6.17mm, respectively). The hydraulic fracture conductivity with proppant propping is the permeability (K) at the reservoir closure pressuref) Width of supporting crack (W)f) 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.
In addition, from the results in table 1, it can be seen that comparative example 1, in which two powder materials were not chemically modified, provided a proppant having significantly lower performance indexes such as fracture rate and amount of deformation of the packed layer than example 5, in which two powder materials were chemically modified.
In addition, after the proppants provided in examples 1 to 5 were placed in an oven at 160 ℃ and heated for 30 days, the fracture rate and compression deformation amount tests were performed 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, and are beneficial to adapting to the downhole environment of deep high-temperature oil and gas wells.
TABLE 2
Example 6
The embodiment provides a resin film coated proppant particle and a preparation method thereof, wherein the proppant particle to be coated is the proppant prepared in embodiment 1, the softening point of phenolic resin in the proppant is 192-197 ℃, and the preparation method specifically comprises the following steps: 20g of a phenol resin prepolymer (Shandong Shengquan New Material Co., Ltd., model 5EXPO974) and 0.6g of propylene carbonate were dissolved in 5g of acetone and stirred uniformly for use (hereinafter referred to as resin solution 1). One-time feeding 500g of the powder with the density of 1.07g/cm into a spraying fluidization device3And fluidizing the composite material ultra-low density proppant particles with the size of 20-100 meshes at an air flow rate of 45L/min. The heating unit of a spray fluidization device (model YC1000 manufactured by shanghai yachen instruments ltd.) was turned on, and the resin solution 1 was sprayed on the surface of the proppant particles with compressed air having a pressure of 0.4MPa while the temperature of the temperature probe at the fluidization site was 80 ℃. After the resin solution 1 is sprayed, the power of a heating unit of the spraying fluidization device is increased, and when the temperature of a temperature probe at the fluidization position is 170 ℃, timing is started and the temperature is kept for 3 min. And then closing a heating unit of the spray fluidization equipment, cooling the product, and sieving to obtain the resin film coated ultra-low density proppant of the embodiment with 20-100 meshes.
Example 7
The embodiment provides a resin film coated proppant particle and a preparation method thereof, wherein the proppant particle to be coated is the proppant prepared in embodiment 2, the softening point of epoxy resin in the proppant is 191-196 ℃, and the preparation method specifically comprises the following steps: 36g of epoxy resin prepolymer (YY 4150, model number of Yijia electronic materials Co., Ltd., Yangcheng, Jiangsu) and 1.2g of n-propylamine were dissolved in 10g of ethanol and stirred uniformly for use (hereinafter referred to as resin solution 2). Fluidization to sprayThe 1000g density of the powder is 1.05g/cm after one-time feeding in the equipment3And fluidizing the composite material ultra-low density proppant particles with the size of 20-100 meshes at an air flow rate of 40L/min. The heating unit of the spray fluidization device (model YC1000 manufactured by shanghai yachen instruments ltd.) was turned on, and the resin solution 2 was sprayed on the surface of the proppant particles with compressed air having a pressure of 0.5MPa while the temperature of the temperature probe at the fluidization site was 90 ℃. After the resin solution 2 was sprayed, the power of the heating unit of the spray fluidizing device was increased, and when the temperature probe at the fluidizing portion was 175 ℃, timing was started and maintained for 5 min. And then closing a heating unit of the spray fluidization equipment, cooling the product, and sieving to obtain the resin film coated ultra-low density proppant of the embodiment with 20-100 meshes.
Example 8
The embodiment provides a resin film coated proppant particle and a preparation method thereof, wherein the proppant particle to be coated is the proppant prepared in embodiment 3, and the softening point of phenolic resin in the proppant is 187-191 ℃. The preparation method comprises the following specific steps: 20g of a polyurethane resin prepolymer (Shandong Shengquan New materials Co., Ltd., model No. PUP0975) and 0.5g of 2,4, 6-tris (dimethylaminomethyl) -phenol were dissolved in 5g of methanol and stirred uniformly for use (hereinafter referred to as a resin solution 3). One-time feeding 500g of the powder with the density of 1.08g/cm into a spraying fluidization device3And fluidizing the composite material ultra-low density proppant particles with the size of 20-100 meshes at an air flow rate of 50L/min. The heating unit of a spray fluidization device (model number YC1000 manufactured by shanghai yachen instruments ltd.) was turned on, and the resin solution 3 was sprayed on the surface of the proppant particles with compressed air having a pressure of 0.5MPa while the temperature of the temperature probe at the fluidization site was 70 ℃. After the resin solution 3 is sprayed, the power of the heating unit of the spray fluidizing device is increased, and when the temperature of the temperature probe at the fluidizing part is 175 ℃, timing is started and maintained for 3 min. And then closing a heating unit of the spray fluidization equipment, cooling the product, and sieving to obtain the resin film coated ultra-low density proppant of the embodiment with 20-100 meshes.
Example 9
The embodiment provides a resin film coated proppant particle and a preparation method thereof, wherein the proppant particle to be coated is the proppant prepared in embodiment 4, and the softening point of epoxy resin in the proppant is 193-197 ℃. The preparation method comprises the following specific steps: 25g of a phenol resin prepolymer (Chongqing Dai synthetic Co., Ltd., model No. PF-10) and 0.6g of ammonium chloride were dissolved in 5g of ethanol, and stirred uniformly for use (hereinafter referred to as a resin solution 4). The 600g of the powder with the density of 1.03g/cm is put into a spraying fluidization device at one time3And fluidizing the composite material ultra-low density proppant particles with the size of 20-100 meshes at an air flow rate of 35L/min. The heating unit of the spray fluidization device (model YC1000 manufactured by shanghai yachen instruments ltd.) was turned on, and the resin solution 4 was sprayed on the surface of the proppant particles with compressed air having a pressure of 0.5MPa while the temperature of the temperature probe at the fluidization site was 80 ℃. After the resin solution 4 is sprayed, the power of a heating unit of the spraying fluidization equipment is increased, and when the temperature of a temperature probe at the fluidization position is 180 ℃, timing is started and the temperature is kept for 3 min. And then closing a heating unit of the spray fluidization equipment, cooling the product, and sieving to obtain the resin film coated ultra-low density proppant of the embodiment with 20-100 meshes.
Example 10
The embodiment provides a resin film coated proppant particle and a preparation method thereof, wherein the proppant to be coated is the proppant prepared in embodiment 5, and the softening point of polyurethane resin in the proppant is 186-190 ℃. The preparation method comprises the following specific steps: 25g of epoxy resin prepolymer (YY 4150, model number of Yijia electronic materials Co., Ltd., Jiangsu salt city) and 0.6g of benzenesulfonic acid were dissolved in 5g of acetone and stirred uniformly until use (hereinafter referred to as resin solution 5). Adding 600g of powder with density of 1.02g/cm into spraying fluidization equipment (model YC1000 manufactured by Shanghai Yachen apparatus Co., Ltd.)3And fluidizing the composite material ultra-low density proppant particles with the size of 20-100 meshes at an air flow rate of 50L/min.
The heating unit of the spray fluidisation apparatus was turned on and the resin solution 5 was sprayed onto the surface of the proppant particles with compressed air at a pressure of 0.5MPa when the temperature probe at the fluidisation point was 80 c. After the resin solution 5 is sprayed, the power of the heating unit of the spray fluidizing device is increased, and when the temperature of the temperature probe at the fluidizing part is 175 ℃, timing is started and kept for 6 min. And then closing a heating unit of the spray fluidization equipment, cooling the product, and sieving to obtain the resin film coated composite material ultra-low density proppant of the embodiment with 20-100 meshes.
The performance test is carried out on the resin film coated high molecular composite material ultra-low density proppant product prepared by the embodiment of the invention, and the breaking rate and the earth acid solubility are both in accordance with the oil and gas industry standard SY/T5108-. The test results of the composite ultra-low density proppant before and after coating with the resin film are shown in table 3 below:
TABLE 3
As can be seen from table 2, the fracture rate of the resin film coated polymer composite proppant particles obtained in the present invention at 52MPa and the solubility in earth acid can be significantly reduced, the former is reduced from about 15% to 18% before coating to about 8% to 9% after coating, and the latter is reduced from about 13% to 14% before coating to about 4% to 5% after coating.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equally replaced; and the modifications or the substitutions do not make the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (28)
1. Resin film coated proppant particleGranules having an apparent density of 1.00 to 1.10g/cm3(ii) a The resin film-coated proppant particles comprise a resin film and proppant particles to be coated, wherein the mass ratio of the resin film to the proppant particles to be coated is 1: 50-3: 50;
the material of the resin film is a reactant of a prepolymer of a second resin and a resin curing accelerator;
the proppant to be coated is 20-100 mesh particles with apparent density of 1.00-1.08 g/cm3The bulk density is 0.40 to 0.50g/m3(ii) a The proppant to be coated comprises a first resin and chemically modified powder which are mutually bonded;
the chemically modified powder comprises a chemically modified first powder and a chemically modified second powder; the first powder material comprises one or more of fly ash and hollow glass microspheres; the second powder material comprises one or more of silicon micropowder and bauxite;
the chemically modified first powder is obtained by chemically modifying a first powder material, and the apparent density of the first powder material is 0.35-0.70 g/cm3The particle size distribution range is 10-90 mu m, and the compressive strength is 40-110 MPa;
the second powder subjected to chemical modification is obtained by chemically modifying a second powder material, and the apparent density of the second powder material is 2.30-3.90g/cm3The particle size distribution range before chemical modification is 2-13 mu m;
the mass ratio of the first resin to the chemically modified first powder to the chemically modified second powder is 40-60: 25-38: 15-20;
the chemical modification refers to the treatment of the first powder material and the second powder material by using modifier alkali and dialdehyde.
2. The resin film-coated proppant particle of claim 1, wherein the base comprises sodium hydroxide and/or potassium hydroxide and the dialdehyde comprises glutaraldehyde and/or succinaldehyde.
3. The resin film-coated proppant particle according to claim 2, wherein the mass ratio of alkali to dialdehyde is 1 to 3: 3 to 1.
4. The resin film-coated proppant particle of claim 1, wherein the first powder material has a median particle diameter D prior to chemical modification50Is 48 μm.
5. The resin film-coated proppant particle according to claim 4, wherein the heat-resistant temperature of the first powder material before chemical modification is not less than 500 ℃.
6. The resin film-coated proppant particle of claim 1, wherein the second powder material has a median particle diameter D prior to chemical modification50And 8 μm.
7. The resin film-coated proppant particle of claim 6, wherein the second powder material has a heat resistance temperature of not less than 500 ℃ before chemical modification.
8. The resin film-coated proppant particle of claim 1, wherein the first resin comprises one or more of an epoxy resin, a phenolic resin, and a polyurethane resin.
9. The resin film-coated proppant particle of claim 1, wherein the proppant to be coated is prepared by:
uniformly mixing the first powder material and the second powder material to obtain a mixed powder material;
adding the modifier into the mixed powder material, and then modifying at a preset temperature and a preset time to obtain a mixed powder of chemically modified first powder and chemically modified second powder;
adding the mixed powder, the prepolymer of the first resin and the first organic solvent into a granulator for binding granulation to obtain granules;
and drying, solidifying, cooling and sieving the obtained granules to obtain the proppant to be coated.
10. The resin film-coated proppant particle according to claim 9, wherein the ratio of the total weight of the modifier to the weight of the first powder material or the second powder material is (1:200) to (1: 10).
11. The resin film-coated proppant particle of claim 9, wherein the first organic solvent comprises one or more of methanol, ethanol, and acetone.
12. The resin film-coated proppant particle according to claim 9, wherein the weight ratio of the prepolymer of the first resin to the first organic solvent is 15 to 20:1 to 2.
13. The resin film-coated proppant particle according to claim 9, wherein the predetermined temperature is 60 to 120 ℃.
14. The resin film-coated proppant particle according to claim 13, wherein the predetermined temperature is 70 to 90 ℃.
15. The resin film-coated proppant particle according to claim 9, wherein the predetermined time is 1 to 6 hours.
16. The resin film-coated proppant particle according to claim 15, wherein the predetermined time is 2 to 3 hours.
17. The resin film-coated proppant particle according to claim 9, wherein the drying temperature is 60 to 100 ℃ and the drying time is 10 to 30 minutes.
18. The resin film-coated proppant particle according to claim 1, wherein the mass ratio of the prepolymer of the second resin to the resin curing accelerator is 70 to 88:2 to 5.
19. The resin film-coated proppant particle of claim 1, wherein the prepolymer of the second resin comprises one or more of a phenolic prepolymer, an epoxy prepolymer, and a polyurethane prepolymer.
20. The resin film-coated proppant particle of claim 1, wherein the resin cure accelerator comprises one or more of ammonium chloride, n-propylamine, benzenesulfonic acid, 2,4, 6-tris (dimethylaminomethyl) -phenol, and propylene carbonate.
21. The method for preparing the resin film-coated proppant particle as set forth in any one of claims 1 to 20, comprising the steps of:
spraying a solution of a prepolymer of a second resin and a resin curing accelerator dissolved in a second organic solvent onto the surface of the proppant particles to be coated at a temperature below the softening point of the proppant particles to be coated, and then drying, curing and sieving to obtain the resin film-coated proppant particles;
the second organic solvent comprises one or more of ethanol, methanol and acetone.
22. The method of claim 21, wherein the proppant particles to be coated are first fluidized with a fluid using a spray fluidizing device, then the fluid is raised in temperature, and a solution of a prepolymer of a second resin and a resin cure promoter dissolved in a second organic solvent is sprayed onto the surface of the proppant particles to be coated using a pressurized gas; and after spraying, raising the temperature of the fluid to carry out fluidization and solidification, thus obtaining the proppant particles coated by the resin film.
23. The preparation method according to claim 22, wherein when the first resin is one or more of an epoxy resin, a phenolic resin and a polyurethane resin, the increasing of the fluid temperature is increasing the fluid temperature to 60-100 ℃; the temperature of the fluid is increased to 150-180 ℃ for fluidization and solidification for 2-10 min.
24. The method of claim 23, wherein the fluidizing the to-be-coated proppant particles with a fluid is to feed the to-be-coated proppant particles to the fluidizing spray apparatus in a formulated amount at a time, and fluidizing them with an air flow rate of 10-50L/min.
25. The preparation method according to claim 22, wherein the spraying of the solution of the prepolymer of the second resin and the resin curing accelerator dissolved in the second organic solvent onto the surface of the proppant particle to be coated with the pressurized gas is performed by spraying the solution of the prepolymer of the second resin and the resin curing accelerator dissolved in the second organic solvent onto the surface of the proppant particle to be coated with compressed air at a pressure of 0.2 to 0.5 MPa.
26. The production method according to any one of claims 21 to 25, wherein the second resin comprises 70 wt.% to 88 wt.% of the prepolymer of the second resin, 10 wt.% to 28 wt.% of the second organic solvent, and 2 wt.% to 5 wt.% of the resin curing accelerator, based on the total weight of the solution of the prepolymer of the second resin and the resin curing accelerator dissolved in the second organic solvent.
27. The preparation method of claim 26, wherein the mass ratio of the solution of the second resin prepolymer and the resin curing accelerator dissolved in the second organic solvent to the proppant particles to be coated is 1-4: 45-55.
28. Use of the resin film coated proppant particle of any one of claims 1 to 20 as a proppant in hydraulic fracture modification.
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| CN115678534B (en) * | 2021-07-29 | 2024-03-19 | 中国石油化工股份有限公司 | Propping agent and preparation method and application thereof |
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