CN117363337A - Preparation process of petroleum fracturing propping agent based on solid waste - Google Patents
Preparation process of petroleum fracturing propping agent based on solid waste Download PDFInfo
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- CN117363337A CN117363337A CN202311669248.2A CN202311669248A CN117363337A CN 117363337 A CN117363337 A CN 117363337A CN 202311669248 A CN202311669248 A CN 202311669248A CN 117363337 A CN117363337 A CN 117363337A
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- propping agent
- solid waste
- fracturing propping
- ceramsite
- petroleum fracturing
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 77
- 239000002910 solid waste Substances 0.000 title claims abstract description 37
- 239000003208 petroleum Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000004927 clay Substances 0.000 claims abstract description 11
- 239000010881 fly ash Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003245 coal Substances 0.000 claims abstract description 9
- 229910000514 dolomite Inorganic materials 0.000 claims abstract description 9
- 239000010459 dolomite Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 39
- 238000007873 sieving Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 10
- -1 heptadecyl-chlorovalerate derivative Chemical class 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 7
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 5
- YSXDKDWNIPOSMF-UHFFFAOYSA-N 5-chloropentanoic acid Chemical compound OC(=O)CCCCCl YSXDKDWNIPOSMF-UHFFFAOYSA-N 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- WTWWTKPAEZQYPW-UHFFFAOYSA-N heptadecan-9-ol Chemical compound CCCCCCCCC(O)CCCCCCCC WTWWTKPAEZQYPW-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 abstract description 13
- 230000004048 modification Effects 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 8
- 230000002209 hydrophobic effect Effects 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 230000000903 blocking effect Effects 0.000 description 10
- 238000011010 flushing procedure Methods 0.000 description 10
- 230000001965 increasing effect Effects 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 230000003075 superhydrophobic effect Effects 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 208000010392 Bone Fractures Diseases 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 206010017076 Fracture Diseases 0.000 description 3
- 239000006004 Quartz sand Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229920001600 hydrophobic polymer Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 210000002489 tectorial membrane Anatomy 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VBGGLSWSRVDWHB-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F VBGGLSWSRVDWHB-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010010214 Compression fracture Diseases 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000008398 formation water Substances 0.000 description 1
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 125000004417 unsaturated alkyl group Chemical group 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention relates to the technical field of compositions for enhancing a cracking effect, and particularly discloses a preparation process of a petroleum fracturing propping agent based on solid waste. The petroleum fracturing propping agent is prepared by crushing, grinding, granulating and sintering flint clay, fly ash, aluminum-containing solid waste, coal gangue and dolomite powder to obtain ceramsite, and performing hydrophobic modification on the ceramsite. The invention also provides a preparation process of the composite. Compared with the prior art, the fracturing propping agent prepared by the method has the advantages of low density, high strength, good water resistance and conductivity and the like.
Description
Technical Field
The invention relates to the technical field of compositions for enhancing a cracking effect, in particular to a preparation process of a petroleum fracturing propping agent based on solid waste.
Background
As an indispensable material in oil and gas exploitation, the fracturing propping agent is pumped into the stratum together with the fracturing fluid in the fracturing work, and plays roles of preventing cracks from closing, increasing the flow guiding rate and increasing the oil and gas resource yield. According to the material quality, the fracturing propping agent can be divided into quartz sand, a tectorial membrane propping agent and a ceramsite propping agent. The quartz sand is taken from the natural world, has the advantages of low cost, easy obtainment and the like, but is only suitable for shallow oil and gas reservoirs due to relatively low compressive strength. The film-coated propping agent is prepared by coating a layer of high-strength polymer material on the surface of quartz sand, so that the compressive strength of the propping agent is improved, but the film-coated process is relatively complex and the preparation period is longer. In contrast, the ceramsite propping agent has the advantages of high strength, low cost, good chemical stability and the like, is easier to support cracks, increases the flow conductivity and achieves the aim of increasing the yield.
The ceramsite is used as a novel functional material and has the characteristics of light weight, heat preservation, high hardness and the like. In recent years, with the development of industry, the application range of ceramsite becomes wide, and the demand is greatly increased. The raw materials for preparing the ceramsite are changed from natural materials such as clay, shale and the like to industrial solid wastes such as building solid wastes, industrial wastes, dressing and smelting solid wastes and the like. Research shows that the components of the dressing and smelting solid wastes have extremely high degree of agreement with the components of the ceramsite raw materials, and the dressing and smelting solid wastes are high-quality raw materials for preparing the ceramsite.
Chinese patent 201410716564.5 provides a preparation method of a super-hydrophobic coated propping agent for oil and gas well fracturing, belongs to the technical field of oil well fracturing material production, and particularly relates to a method for preparing super-hydrophobic ceramic sand by coating a film through a compound reaction of alkylsilane and halosilane. It comprises the following steps: (1) uniformly mixing unsaturated alkyl silane, fluoro silane and hydrogen peroxide, and reacting for 1-4 hours at the temperature of 30-50 ℃ to form a prepolymer; (2) and uniformly mixing hydrogen peroxide and prepolymer in a fluidized bed, uniformly spraying the obtained mixed solution on the surface of aggregate, and carrying out polymerization reaction for 1-2 hours at 60-80 ℃ to obtain the super-hydrophobic tectorial membrane proppant for oil-gas well fracturing. The invention has even and stable reaction, high product quality and good product stability. Uniformly sprayed on the surface of aggregate for polymerization reaction, and has the characteristics of economy, low energy consumption and high yield.
Chinese patent 201610517344.9 discloses a preparation method of a propping agent coated with a super-hydrophobic polymer film, which is characterized in that: mixing an organosilicon precursor and alcohol, regulating the pH value to 12-13 by using alkali liquor, reacting for 0.5-5 hours at the temperature of 30-70 ℃, and then adding fluorosilane for reaction; mixing the reacted liquid and the linear resin, and heating to 70-100 ℃; and adding a curing agent, mixing with the propping agent, curing for 1-3 hours at the temperature of 90-120 ℃, and then heating to 150-200 ℃ for curing for 1-3 hours to obtain the propping agent wrapped with the super-hydrophobic polymer film. According to the invention, the contact angle between the surface of the prepared polymer film and water is larger than 150 degrees, the hydrophobicity of the surface of the propping agent can be greatly improved, and the propping agent modified by the polymer film is used as a key material of a hydraulic fracturing technology, so that the exploitation quality and yield of shale oil gas can be improved, and the practicability is strong.
The conductivity of the fracture is primarily dependent on the amount of permeability provided by the proppant pack in the fracture, and therefore the performance and quality of the proppant becomes a major factor affecting the conductivity of the fracture. The low density and high strength of proppants in the prior art are related to the conductivity, but the consideration of the oil-water infiltration property of the proppants is also of great importance. The oil-water infiltration property of the surface of the propping agent can determine the flow conductivity of the propping agent to oil and water, and the propping agent with hydrophobic surface can form water shutoff and oil drainage pore channels so as to achieve the aim of fracturing and increasing yield. The oil and gas well reformed by the super-hydrophobic fracturing propping agent can improve the recovery ratio by 5-20%. Therefore, in order to meet the requirements of the compression fracture strength of the propping agent in the exploitation process of the oil and gas field and the hydrophobicity of the propping agent in the later period of exploitation, the research on the petroleum fracturing propping agent with high water blocking capacity and low breaking rate has great practical significance.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a process for preparing a petroleum fracturing propping agent based on solid waste.
At present, the method for carrying out hydrophobic modification on the propping agent mainly comprises two modes of physical modification and coating modification, but the micro-nano structure formed by the physical modification is easy to damage, and the surfactant coating is often hydrophobic effect achieved by fluorine-containing substances, so that the environment is easy to be polluted. Therefore, in the invention, the ceramsite propping agent is obtained by mixing various wastes and granulating through sintering, and as the ceramsite is used as an inorganic material, the main component of the ceramsite is various metal and nonmetal oxides, the surface of the ceramsite has rich active hydroxyl groups, and the wettability of the surface of the ceramsite can be changed by modifying the hydrophobicity of the ceramsite, so that the propping agent is endowed with good hydrophobicity, thereby having better water control and flow guide effects and achieving the aim of fracturing and increasing yield. And the surface of the ceramsite is not easy to be soaked by water, so that the ceramsite has better salt resistance and flushing resistance, and the propping agent has longer service life.
In order to achieve the above purpose, the invention provides a preparation process of a petroleum fracturing propping agent based on solid waste, which comprises the following steps:
s1: mixing and crushing 300-600 parts by weight of flint clay, 100-200 parts by weight of fly ash, 50-100 parts by weight of aluminum-containing solid waste, 100-150 parts by weight of coal gangue and 50-80 parts by weight of dolomite, grinding and sieving with a 300-mesh sieve to obtain a dry material;
s2: spraying and granulating the dry materials, screening raw material balls, sieving with a 20-40 mesh sieve, drying at 100-120 ℃ to constant weight, sintering at 1300-1400 ℃ for 2-3 hours, cooling to room temperature, and sieving with a 30-40 mesh sieve for the second time to obtain a ceramsite proppant;
s3: adding 10-15 parts by weight of 5-chlorovaleric acid into 200-400 parts by weight of dichloromethane, cooling to 0-5 ℃, adding 12-14 parts by weight of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 15-18 parts by weight of triethylamine and 0.4-0.8 part by weight of 4-dimethylaminopyridine in a nitrogen atmosphere, and uniformly stirring to obtain a solution A; adding 20-30 parts by weight of heptadecan-9-ol into 150-300 parts by weight of dichloromethane to obtain a solution B; dropwise adding the solution B into the solution A, stirring at room temperature for 20-30 hours after the dropwise adding, adding water for quenching, separating liquid, washing a water phase by methylene dichloride, separating liquid, merging an organic phase, concentrating under reduced pressure to obtain a residue, adding a saturated sodium bicarbonate aqueous solution for washing, extracting by using ethyl acetate, and concentrating the organic phase under reduced pressure after separating liquid to obtain the heptadecyl-chlorovalerate derivative;
s4: and adding 100-200 parts by weight of ceramsite propping agent into 1000-2000 parts by weight of N, N-dimethylformamide, adding 15-30 parts by weight of heptadecyl-chlorovalerate derivative, heating to 80-100 ℃, stirring for 2-6 hours, filtering, and drying ceramsite to obtain the ceramsite.
Further, in the step S1, the calcination temperature is 800-1200 ℃ and the calcination time is 2-4 hours.
Further, in the step S2, the temperature rising rate during sintering is 5 ℃/min.
The invention also provides a solid waste-based petroleum fracturing propping agent which is prepared by the process.
The invention has the beneficial effects that:
1. compared with the prior art, the fracturing propping agent prepared by the method has good hydrophobic property, good water resistance, obvious selective water control effect and excellent salt resistance and flushing resistance.
2. According to the invention, the wettability of the surface of the ceramic particles can be changed by modifying the hydrophobicity of the ceramic particles, so that good hydrophobicity is given to the propping agent, a better water control and flow guide effect is achieved, and the aim of fracturing and yield increasing is achieved. And the surface of the ceramsite is not easy to be soaked by water, so that the ceramsite has better salt resistance and flushing resistance, and the propping agent has longer service life.
3. According to the invention, flint clay, fly ash, solid waste containing aluminum, coal gangue and dolomite are used as raw materials, and sintered to obtain the ceramsite proppant, so that the obtained proppant has the characteristics of low density and high strength, and the proppant subjected to hydrophobic modification also has good hydrophobicity and lipophilicity, so that the oil yield of crude oil is improved, and the exploitation of petroleum is facilitated. The invention uses solid waste as raw materials, thereby changing waste into valuables, reducing cost and having great application value.
Detailed Description
Comparative example 1
A preparation process of a petroleum fracturing propping agent based on solid waste comprises the following steps:
s1: 5kg of flint clay is calcined at 1000 ℃ for 3 hours, then mixed and crushed with 1.5kg of fly ash, 0.8kg of aluminum-containing solid waste, 1.2kg of coal gangue and 0.6kg of dolomite, and ground and sieved by a 300-mesh sieve to obtain a dry material;
s2: and (3) spraying and granulating the dry materials, screening raw material balls, sieving the raw material balls by a 20-mesh sieve, drying the raw material balls at 100 ℃ until the weight is constant, sintering the raw material balls at 1350 ℃ for 3 hours, heating the raw material balls at a speed of 5 ℃/min during sintering, cooling the raw material balls to room temperature, and sieving the raw material balls by a 30-mesh sieve for the second time.
Example 1
A preparation process of a petroleum fracturing propping agent based on solid waste comprises the following steps:
s1: 5kg of flint clay is calcined at 1000 ℃ for 3 hours, then mixed and crushed with 1.5kg of fly ash, 0.8kg of aluminum-containing solid waste, 1.2kg of coal gangue and 0.6kg of dolomite, and ground and sieved by a 300-mesh sieve to obtain a dry material;
s2: spraying and granulating the dry materials, sieving raw material balls, sieving with a 20-mesh sieve, drying at 100 ℃ to constant weight, sintering at 1350 ℃ for 3 hours, heating at a rate of 5 ℃/min during sintering, cooling to room temperature, and sieving with a 30-mesh sieve for the second time to obtain the ceramsite propping agent;
s3: adding 0.12kg of 5-chlorovaleric acid into 3L of dichloromethane, cooling to 0 ℃, adding 0.13kg of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 0.16kg of triethylamine and 6g of 4-dimethylaminopyridine under nitrogen atmosphere, and uniformly stirring to obtain a solution A; 0.25kg of heptadec-9-ol was added to 2.5L of dichloromethane to obtain a solution B; dropwise adding the solution B into the solution A, stirring at room temperature for 25 hours after the dropwise adding, adding water for quenching, separating liquid, washing a water phase by methylene dichloride, separating liquid, merging organic phases, concentrating under reduced pressure to obtain a residue, adding a saturated sodium bicarbonate aqueous solution for washing, extracting by using ethyl acetate, and concentrating the organic phase under reduced pressure after separating liquid to obtain the heptadecyl-chlorovalerate derivative;
s4: adding 1.5kg of ceramsite propping agent into 15L of N, N-dimethylformamide, adding 0.2kg of heptadecyl-chlorovalerate derivative, heating to 90 ℃ and stirring for 4 hours, filtering, and drying ceramsite to obtain the ceramsite.
Example 2
A preparation process of a petroleum fracturing propping agent based on solid waste comprises the following steps:
s1: 5kg of flint clay is calcined at 1000 ℃ for 3 hours, then mixed and crushed with 1.5kg of fly ash, 0.8kg of aluminum-containing solid waste, 1.2kg of coal gangue and 0.6kg of dolomite, and ground and sieved by a 300-mesh sieve to obtain a dry material;
s2: spraying and granulating the dry materials, sieving raw material balls, sieving with a 20-mesh sieve, drying at 100 ℃ to constant weight, sintering at 1350 ℃ for 3 hours, heating at a rate of 5 ℃/min during sintering, cooling to room temperature, and sieving with a 30-mesh sieve for the second time to obtain the ceramsite propping agent;
s3: adding 40g of ethyl orthosilicate into 400mL of ethanol, regulating the pH to 12 by using 1mol/L ammonia water, stirring for 2 hours at 50 ℃, adding 5g of perfluorodecyl trimethoxy silane, continuously stirring for 2 hours, mixing with 7.5g of phenolic resin, heating to 70 ℃, stirring and mixing uniformly, adding 0.75g of urotropine, mixing and stirring uniformly with 1.5kg of ceramsite propping agent for 30 minutes, wrapping a layer of super-hydrophobic polymer film on the surface of ceramsite, and solidifying for 6 hours at 120 ℃ to obtain the modified porous ceramic.
Example 3
A preparation process of a petroleum fracturing propping agent based on solid waste comprises the following steps:
s1: 5kg of flint clay is calcined at 1000 ℃ for 3 hours, then mixed and crushed with 1.0kg of fly ash, 0.8kg of aluminum-containing solid waste, 1.2kg of coal gangue and 0.6kg of dolomite, and ground and sieved by a 300-mesh sieve to obtain a dry material;
s2: spraying and granulating the dry materials, sieving raw material balls, sieving with a 20-mesh sieve, drying at 100 ℃ to constant weight, sintering at 1350 ℃ for 3 hours, heating at a rate of 5 ℃/min during sintering, cooling to room temperature, and sieving with a 30-mesh sieve for the second time to obtain the ceramsite propping agent;
s3: adding 0.12kg of 5-chlorovaleric acid into 3L of dichloromethane, cooling to 0 ℃, adding 0.13kg of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 0.16kg of triethylamine and 6g of 4-dimethylaminopyridine under nitrogen atmosphere, and uniformly stirring to obtain a solution A; 0.25kg of heptadec-9-ol was added to 2.5L of dichloromethane to obtain a solution B; dropwise adding the solution B into the solution A, stirring at room temperature for 25 hours after the dropwise adding, adding water for quenching, separating liquid, washing a water phase by methylene dichloride, separating liquid, merging organic phases, concentrating under reduced pressure to obtain a residue, adding a saturated sodium bicarbonate aqueous solution for washing, extracting by using ethyl acetate, and concentrating the organic phase under reduced pressure after separating liquid to obtain the heptadecyl-chlorovalerate derivative;
s4: adding 1.5kg of ceramsite propping agent into 15L of N, N-dimethylformamide, adding 0.2kg of heptadecyl-chlorovalerate derivative, heating to 90 ℃ and stirring for 4 hours, filtering, and drying ceramsite to obtain the ceramsite.
Example 4
A preparation process of a petroleum fracturing propping agent based on solid waste comprises the following steps:
s1: 5kg of flint clay is calcined at 1000 ℃ for 3 hours, then mixed and crushed with 2kg of fly ash, 0.8kg of aluminum-containing solid waste, 1.2kg of coal gangue and 0.6kg of dolomite, and ground and sieved by a 300-mesh sieve to obtain a dry material;
s2: spraying and granulating the dry materials, sieving raw material balls, sieving with a 20-mesh sieve, drying at 100 ℃ to constant weight, sintering at 1350 ℃ for 3 hours, heating at a rate of 5 ℃/min during sintering, cooling to room temperature, and sieving with a 30-mesh sieve for the second time to obtain the ceramsite propping agent;
s3: adding 0.12kg of 5-chlorovaleric acid into 3L of dichloromethane, cooling to 0 ℃, adding 0.13kg of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 0.16kg of triethylamine and 6g of 4-dimethylaminopyridine under nitrogen atmosphere, and uniformly stirring to obtain a solution A; 0.25kg of heptadec-9-ol was added to 2.5L of dichloromethane to obtain a solution B; dropwise adding the solution B into the solution A, stirring at room temperature for 25 hours after the dropwise adding, adding water for quenching, separating liquid, washing a water phase by methylene dichloride, separating liquid, merging organic phases, concentrating under reduced pressure to obtain a residue, adding a saturated sodium bicarbonate aqueous solution for washing, extracting by using ethyl acetate, and concentrating the organic phase under reduced pressure after separating liquid to obtain the heptadecyl-chlorovalerate derivative;
s4: adding 1.5kg of ceramsite propping agent into 15L of N, N-dimethylformamide, adding 0.2kg of heptadecyl-chlorovalerate derivative, heating to 90 ℃ and stirring for 4 hours, filtering, and drying ceramsite to obtain the ceramsite.
Test example 1
The proppant obtained in the comparative examples and examples was tested for bulk density, crush rate according to the proppant performance test method for SY/T5108-2014 hydraulic fracturing and gravel packing operations. The contact angle test is to lay the proppants on a glass sheet, and to measure the water contact angle of the surface after fixing. And testing the water blocking performance of the propping agent by adopting the propping agent water blocking height measuring device. The method comprises the following specific steps: taking transparent glass tubes with openings at the upper end and the lower end and inner diameters of 50mm, vertically fixing the transparent glass tubes on an iron stand, and installing a screen at the lower end; adding a proppant sample to the glass tube to a height of 10 cm; slowly adding water into the propping agent sand bed in the glass tube; when water begins to flow out of the screen at the bottom of the proppant sand bed, the water level in the glass tube is recorded to characterize the water blocking properties of the proppant. The test results are shown in Table 1.
TABLE 1 proppant mechanics and Water blocking test results table
As can be seen from the performance test of the proppants, the proppants obtained by the invention have the characteristics of low density and high strength, and the comparison of the examples 1 and 3-4 shows that the porous structure of the fly ash can cause the density of the proppants to be reduced but the crushing rate to be increased at the same time when the addition amount of the fly ash is increased, so that the addition amount of the proppants is proper.
The wettability of the propping agent has a remarkable influence on oil-water seepage, when the surface of the propping agent is changed from hydrophilicity to neutrality and lipophilicity, the water-phase seepage resistance is greatly increased, and the oil-phase seepage resistance is reduced. Contact angle is one of the main characterizing parameters of wettability. From hydrophobicity and water resistance tests, it can be found that in the embodiment, hydrophilic ceramsite is successfully converted into hydrophobicity through hydrophobic modification on the ceramsite proppant, so that the proppant in comparative example 1 is not only hydrophobic but also has no water resistance, and in the embodiment, the proppant is endowed with hydrophobicity through physical coating modification or chemical grafting modification, so that the proppant has better water control and flow guide effects, and the aim of fracturing and yield increase can be achieved.
The water blocking height is an important index for evaluating the water control performance of the water control propping agent, and has the characteristics of intuitiveness, rapidness and good repeatability. The proppant in example 1 had a water blocking height of 25cm and had a remarkable water blocking effect, whereas the proppant in comparative example 1 had no water blocking property and a water blocking height of 0. Tests show that the prepared hydrophobic propping agent can delay water breakthrough time and reduce the water flow speed after water breakthrough, thereby playing a role in controlling water. Meanwhile, water can not be adsorbed on the surface of the propping agent in a water binding mode after flowing through the propping agent filling layer, so that the influence of water binding is reduced, and the recovery ratio is improved.
Test example 2
The proppants in the examples were tested for flushing and salt resistance. The propping agent is filled into a sand filling pipe with the size of phi 38mm multiplied by 300mm, the flow rate is set to be 10L/min, the stratum water is used for continuous flushing for 7d by adopting a horizontal flow pump, and then the water contact angle test is carried out. The proppants were placed in 200g/L aqueous sodium chloride solution and soaked for 7d. And (5) taking out and drying, measuring the contact angle of the surface of the propping agent, and comparing with the contact angle before soaking. The specific data are shown in Table 2.
TABLE 2 results of the proppant washout resistance and salt resistance test
After the proppant pack is completed, it is subjected to flushing of formation fluids for a long period of time. The flushing resistance test can well simulate the flowing condition of formation fluid in a well bore. From the test results, the proppants in examples 1 and 3-4 can still keep stable wettability after being continuously washed for 7d and soaked in a salt solution for 7d. The preparation method is probably because grafting modification is carried out on the surface of the ceramsite, and the polymer chains are bonded with the surface of the ceramsite through covalent bond action, so that a more stable modification effect is achieved, and even though the surface grafting layer of the propping agent is eroded by stratum water at a high speed continuously and is not stripped or destroyed, the surface grafting layer of the propping agent is firmly combined with the matrix, and the preparation method can withstand the continuous flushing of fluid and the environment of the saline solution under stratum conditions, so that the water control effective period is ensured.
In example 2, the surface of the ceramsite is subjected to film coating modification, so that the resin and the surface of the ceramsite are not chemically reacted and are connected only by physical action, and the fact that the binding force between the surface coating layer and the propping agent aggregate is weak is caused. The proppant surface coating may be in danger of desorption under the condition of flushing of formation water and saline solution. Meanwhile, the porous particles have poor surface coating effect due to the attraction of capillary force, and thus the proppant in example 2 has inferior flushing and salt resistance as compared with examples 1 and 3 to 4.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (10)
1. A preparation process of a petroleum fracturing propping agent based on solid waste comprises the following steps:
s1: calcining flint clay, mixing and crushing the flint clay, fly ash, aluminum-containing solid waste, coal gangue and dolomite, and grinding and sieving the mixture to obtain a dry material;
s2: spraying and granulating the dry materials, sieving raw material balls, drying to constant weight after sieving, sintering and preserving heat, cooling to room temperature, and secondarily sieving to obtain a ceramsite propping agent;
s3: adding 5-chlorovaleric acid into dichloromethane, cooling to 0-5 ℃, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, triethylamine and 4-dimethylaminopyridine in a nitrogen atmosphere, and uniformly stirring to obtain a solution A; heptadecane-9-ol is added into methylene dichloride to obtain solution B; dropwise adding the solution B into the solution A, stirring at room temperature for 20-30 hours after the dropwise adding, adding water for quenching, separating liquid, washing a water phase by methylene dichloride, separating liquid, merging an organic phase, concentrating under reduced pressure to obtain a residue, adding a saturated sodium bicarbonate aqueous solution for washing, extracting by using ethyl acetate, and concentrating the organic phase under reduced pressure after separating liquid to obtain the heptadecyl-chlorovalerate derivative;
s4: adding the ceramsite propping agent into N, N-dimethylformamide, adding the heptadecyl-chlorovalerate derivative, heating and stirring for 2-6 hours, filtering, and drying the ceramsite to obtain the ceramsite.
2. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: in the step S1, the calcination temperature is 800-1200 ℃ and the calcination time is 2-4 hours.
3. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: the sieving grain size in the step S1 is 300 meshes.
4. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: the sintering temperature in the step S2 is 1300-1400 ℃, and the temperature rising rate during sintering is 5 ℃/min.
5. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: and in the step S2, the sintering and heat preservation time is 2-3 hours.
6. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: and the particle size of the first screening in the step S2 is 20-40 meshes.
7. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: and the temperature of drying in the step S2 is 100-120 ℃.
8. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: and in the step S2, the particle size of the second screening is 30-40 meshes.
9. The process for preparing the solid waste-based petroleum fracturing propping agent, as claimed in claim 1, is characterized in that: and in the step S4, the heating and stirring temperature is 80-100 ℃.
10. A solid waste-based petroleum fracturing propping agent, which is characterized by being prepared by the process of any one of claims 1-9.
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