WO2025002097A1 - 一种缓解套管变形的水泥浆体系及其制备方法和应用 - Google Patents

一种缓解套管变形的水泥浆体系及其制备方法和应用 Download PDF

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Publication number
WO2025002097A1
WO2025002097A1 PCT/CN2024/101215 CN2024101215W WO2025002097A1 WO 2025002097 A1 WO2025002097 A1 WO 2025002097A1 CN 2024101215 W CN2024101215 W CN 2024101215W WO 2025002097 A1 WO2025002097 A1 WO 2025002097A1
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Prior art keywords
cement slurry
alleviating
slurry system
casing deformation
cement
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English (en)
French (fr)
Inventor
张晓兵
张华�
张弛
于永金
齐奉忠
曲从锋
张顺平
丁志伟
郭雪利
张佳滢
徐璞
张海志
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Cnpc Engineering Technology R & D Co Ltd
China National Petroleum Corp
CNPC Engineering Technology R&D Co Ltd
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Cnpc Engineering Technology R & D Co Ltd
China National Petroleum Corp
CNPC Engineering Technology R&D Co Ltd
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Publication of WO2025002097A1 publication Critical patent/WO2025002097A1/zh
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/428—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for squeeze cementing, e.g. for repairing
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
    • 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
    • E21B33/00—Sealing or packing boreholes or wells
    • E21B33/10—Sealing or packing boreholes or wells in the borehole
    • E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/08—Fiber-containing well treatment fluids

Definitions

  • the invention relates to the technical field of shale gas cementing, and in particular to a cement slurry system for alleviating casing deformation, and a preparation method and application thereof.
  • CN202210052442.5 discloses a high-density anti-channeling tough cement slurry system for shale gas cementing, and its preparation method and application, which includes G-grade cement, water, composite weighting agent, nano anti-channeling agent, toughening agent, fluid loss reducer, retarder, dispersant and defoaming agent.
  • the addition of nano anti-channeling agent not only has no negative impact on the construction performance of cement slurry, but also can promote the formation of early strength of cement, reduce the permeability of cement stone, make the structure of cement stone more uniform and dense, and effectively enhance the anti-channeling property of cement stone.
  • CN201910113067.9 discloses a cementing slurry system suitable for large-scale staged fracturing of shale gas horizontal wells, which mainly includes 100 parts of oil well cement, 43-46 parts of fresh water, 2-4 parts of elastic and toughening agent, 1-2 parts of anti-channeling agent, 1-3 parts of fluid loss reducer, 0.4-0.6 parts of dispersant, 1-1.5 parts of swelling agent, 0.5-2.0 parts of retarder, and 0.1-0.5 parts of defoaming agent.
  • the elastic and toughening agent is a rubber fiber with a specific surface area ⁇ 7m/g and a volume compression rate ⁇ 5%, or a mixture of the rubber fiber and rubber particles.
  • the cementing slurry system of this technology has excellent comprehensive properties such as thickening and anti-channeling performance, elasticity and toughness, which can effectively realize the synchronous deformation of the cement ring and casing when the cement ring is subjected to the alternating load of staged fracturing, ensuring the long-term integrity of the wellbore seal of the shale gas horizontal well during the later reservoir transformation and gas trial production operations, effectively preventing the occurrence of casing annulus pressure, and providing effective guarantee for the long-term production and large-scale fracturing of shale gas horizontal wells.
  • CN201410471036.8 discloses a toughening and anti-channeling agent for cement and toughening cement for shale gas horizontal well cementing.
  • the technology relates to a cement slurry used in shale gas horizontal well cementing and a toughening additive added therein.
  • the toughening and anti-channeling agent for cement is prepared by mixing styrene-butadiene rubber powder and redispersible latex powder in a mass ratio of 2:1, wherein the The styrene butadiene rubber powder was treated as follows before use: firstly, a silane coupling agent solution with a mass percentage of 1.5% was prepared, and the styrene butadiene rubber powder was added thereto, and the solution was filtered after standing for 24 hours, and the cement slurry was dried in the sun, and the system performance was stable, the thickening time was easy to adjust, the water loss was less than 30ml, the free liquid at a 45-degree inclination angle and the upper and lower density differences were both 0.50°C, the compressive strength was greater than 30Mpa for 24h, the applicable temperature range was 50-120°C, and the thickening time was 110-240min; the toughened cement for shale gas horizontal well cementing was added with the above-mentioned toughening and anti
  • the present invention provides a cement slurry system for alleviating casing deformation and a preparation method thereof.
  • the cement slurry system has low finished product cost and is easy to prepare.
  • the present invention provides a cement slurry system for relieving casing deformation, wherein the raw materials include G-grade oil well cement and other raw materials in the following percentages based on the mass of G-grade oil well cement: 3-6% microsilicon, 15-50% glass microspheres, 3-6% reinforcing material, 3-5% toughening material, 0-2% stabilizer, 0-2.5% dispersant, 3-6% fluid loss reducer, 0-2.5% retarder, 0.2-0.5% defoamer, 0.2-0.5% antifoamer, and 70-95% water;
  • the toughening material is compounded by fibers and carbon materials in a mass ratio of 2-4:1, the fibers include one or a combination of two or more of basalt fibers, alumina fibers, and silicon carbide fibers, and the carbon materials include carbon nanotubes and/or expanded graphite;
  • the compressive strength of the glass microspheres is 3000-5000 psi.
  • the raw materials of the cement slurry system for alleviating casing deformation include, by weight: 100 parts of G-grade oil well cement, 3-6 parts of microsilicon, 15-50 parts of glass microspheres, 3-6 parts of reinforcing material, 3-5 parts of toughening material, 0-2 parts of stabilizer, 0-2.5 parts of dispersant, 3-6 parts of fluid loss reducer, 0-2.5 parts of retarder, 0.2-0.5 parts of defoamer, 0.2-0.5 parts of antifoaming agent, and 70-95 parts of water;
  • the toughening material is compounded by fibers and carbon materials in a mass ratio of 2-4:1, the fibers include one or a combination of two or more of basalt fibers, alumina fibers, and silicon carbide fibers, and the carbon materials include carbon nanotubes and/or expanded graphite; the compressive strength of the glass microbeads is 3000-5000psi.
  • the compressive strength of the glass microspheres is 4000 psi.
  • the present invention reduces the elastic modulus of cement paste without affecting its compressive strength by adding glass microspheres with low compressive strength and toughening materials made of fiber and carbon materials, so that the compression resistance of cement paste reaches its own compressive resistance limit.
  • the internal glass beads have been broken before the damage occurs, providing a certain buffer space for the casing deformation, and the ability of cement stone to alleviate casing deformation is gradually enhanced.
  • the fiber length of the basalt fiber is 1.5-10 ⁇ m.
  • the fiber length of the alumina fiber is 3-6 ⁇ m.
  • the fiber length of the silicon carbide fiber is 10-15 ⁇ m.
  • the length of the carbon nanotubes is 10-30 ⁇ m.
  • the particle size of the expanded graphite is 40-50 ⁇ m.
  • the average particle size of the microsilica is 4-10 ⁇ m, and the 45 ⁇ m sieve residue is ⁇ 5%.
  • the true density of the glass beads is 0.38-0.42 g/cm 3 , more preferably 0.40 g/cm 3 .
  • the present invention optimizes the true density of the glass beads. When the true density of the glass beads is too large, the space they can provide after being broken is limited.
  • the stabilizer is an ore powder stabilizer and/or a polymer stabilizer, more preferably an ore powder stabilizer.
  • the dispersant is a condensation product of formaldehyde and acetone and/or a polystyrene sulfonate dispersant.
  • the fluid loss reducer is a polyacrylamide-based fluid loss reducer.
  • the retarder is an acrylamide retarder.
  • the defoaming agent includes one or a combination of two or more of tributyl phosphate, polyoxypropylene glycerol, and polydimethylsiloxane.
  • the 7-day compressive strength of the cement paste formed by the cement slurry system for alleviating casing deformation is greater than 20 MPa, and the elastic modulus is less than 5 GPa.
  • the cement slurry system for alleviating casing deformation has a density of 1.30-1.60 g/cm 3 and an applicable temperature range of 30-150°C.
  • the present invention also provides a method for preparing the above-mentioned cement slurry system for alleviating casing deformation, the method comprising: weighing raw materials in proportion and mixing them, stirring them evenly at a speed of 11500-12500 r/min to obtain the cement slurry system for alleviating casing deformation.
  • the method for preparing the cement slurry system for alleviating casing deformation comprises the following steps:
  • the dry mix is evenly poured into the wet mix solution.
  • the stirrer speed is adjusted to 11500-12500 r/min, and stirring is continued to obtain the cement slurry system for alleviating casing deformation.
  • the present invention also provides an application of the above-mentioned cement slurry system for alleviating casing deformation in cementing shale gas wells and preventing and/or alleviating casing deformation.
  • the cement slurry system for relieving casing deformation provided by the present invention meets the requirements of cementing construction.
  • the cement stone has a low elastic modulus, and can actively break to exchange space when the formation slip is large, providing space for casing deformation, and has a good effect of preventing and relieving casing deformation.
  • the 7-day compressive strength of the cement stone formed by the cement slurry system for relieving casing deformation of the present invention is greater than 20MPa, and the elastic modulus is less than 5GPa.
  • G-grade oil well cement is high sulfate resistance (HSR) G-grade oil well cement, produced by Dalian Cement Group Co., Ltd.;
  • the stabilizer is a mature product produced by China National Petroleum Corporation Engineering Technology Research Institute Co., Ltd., and its trade name is "DRB-1S, a reinforcing material ore powder for oil well cementing".
  • Basalt fibers are commercially available with a fiber length of 1.5-10 ⁇ m;
  • Alumina fibers are commercially available with a fiber length of 3-6 ⁇ m;
  • the length of silicon carbide fiber is 10-15 ⁇ m
  • Carbon nanotubes 95% purity, 10-30 ⁇ m in length
  • Expanded graphite is commercially available with a purity of more than 95% and a particle size of 48 ⁇ m (mesh number 300 mesh);
  • Microsilica is commercially available with an average particle size of 5 ⁇ m and a 45 ⁇ m sieve residue of ⁇ 5%;
  • the dispersant is a condensation product of formaldehyde and acetone or a polystyrene sulfonate dispersant
  • Fluid loss reducer is a type of polyacrylamide
  • the defoaming agent is one of tributyl phosphate, polyoxypropylene glycerol and polydimethylsiloxane commonly used in the art.
  • This embodiment provides a cement slurry system for alleviating casing deformation, and the preparation method thereof is as follows:
  • the cement slurry formula is as follows by weight percentage: 100 parts of G-grade oil well cement, 5 parts of microsilicon, 10 parts of reinforcing material, 4 parts of toughening material, 13 parts of glass microspheres, 1 part of stabilizer, 1.5 parts of dispersant, 3.5 parts of fluid loss reducer, 0.8 parts of retarder, 0.5 parts of defoamer, 0.5 parts of antifoaming agent, and 70 parts of water; wherein the toughening material is formed by uniformly stirring 2 parts of basalt fiber and 1 part of expanded graphite; the true density of the glass microspheres is 0.40 g/cm 3 and the compressive strength is 4000 psi.
  • This embodiment provides a cement slurry system for alleviating casing deformation, and the preparation method thereof is as follows:
  • the cement slurry formula is as follows by weight percentage: 100 parts of G-grade oil well cement, 5 parts of microsilicon, 10 parts of reinforcing material, 4 parts of toughening material, 32 parts of glass microspheres, 1 part of stabilizer, 1.5 parts of dispersant, 3.5 parts of fluid loss reducer, 0.8 parts of retarder, 0.5 parts of defoamer, 0.5 parts of antifoaming agent, and 75 parts of water; wherein the toughening material is formed by uniformly stirring 3 parts of silicon carbide fiber and 1 part of expanded graphite; the true density of the glass microspheres is 0.40 g/cm 3 and the compressive strength is 4000 psi.
  • the preparation method is the same as that of Example 1.
  • the density of the cement slurry is 1.45 g/cm 3 .
  • This embodiment provides a cement slurry system for alleviating casing deformation, and the preparation method thereof is as follows:
  • the cement slurry formula is as follows by weight percentage: 100 parts of G-grade oil well cement, 5 parts of microsilicon, 10 parts of reinforcing material, 4 parts of toughening material, 50 parts of glass microspheres, 1 part of stabilizer, 1.5 parts of dispersant, 3.5 parts of fluid loss reducer, 0.8 parts of retarder, 0.5 parts of defoamer, 0.5 parts of antifoaming agent, and 78 parts of water; wherein the toughening material is formed by uniformly stirring 4 parts of alumina fiber and 1 part of carbon nanotube; the true density of the glass microspheres is 0.40g/ cm3 , and the compressive strength is 4000psi.
  • the preparation method is the same as that of Example 1.
  • the density of the cement slurry is 1.3 g/cm 3 .
  • This comparative example provides a cement slurry system, whose formula and preparation method are the same as those of Example 1, except that no toughening material is added in this comparative example, the true density of the glass microspheres used is 0.63 g/cm 3 , and the compressive strength is 15000 psi; meanwhile, in order to keep the density of the cement slurry unchanged, the weight fraction of water is changed to 68 parts.
  • This comparative example provides a cement slurry system, whose formula and preparation method are the same as those of Example 2, except that no toughening material is added in this comparative example, and the true density of the glass microspheres is 0.60 g/cm 3 and the compressive strength is 12000 psi; meanwhile, in order to keep the density of the cement slurry unchanged, the weight fraction of water is changed to 73 parts.
  • This comparative example provides a cement slurry system, whose formula and preparation method are the same as those of Example 3, except that no toughening material is added in this comparative example, and the true density of the glass microspheres is 0.60 g/cm 3 and the compressive strength is 12000 psi; meanwhile, in order to keep the density of the cement slurry unchanged, the weight fraction of water is changed to 76 parts.
  • the main experimental instruments are: 30-60 type tile stirrer; TG7370D type pressurized curing kettle, Shenyang Tiger Petroleum Instrument Equipment Manufacturing Co., Ltd.; HH-420 type constant temperature digital display water tank, Changzhou Yineng Experimental Instrument Factory; YAW-300B hydraulic pressure testing machine, Jinan Xinshijin Testing Machine Co., Ltd.
  • This experimental example also uses the following method to test the breakage rate of glass beads under specified conditions:
  • the crushing rate is determined based on the change in density before and after compression of the sample under a specified pressure.
  • ⁇ 1 density of the sample before compression, g/cm 3 ;
  • the fluidity of the cement slurry systems of Examples 1-3 is greater than 20 cm, and the API water loss is less than 50 mL, which meets the requirements of cementing construction; the 7-day compressive strength of the cement stone formed by the cement slurry systems of Examples 1-3 is greater than 20 MPa, and the elastic modulus is less than 5 GPa, with good performance, meeting the cementing sealing requirements.
  • Example 2 Compared with Comparative Example 2, after adding toughening material and replacing glass beads with a compressive strength of 4000pasi in Example 2, the conventional properties of the cement slurry such as API water loss, fluidity, and compressive strength of the two do not change much, and both meet the construction requirements; however, the elastic modulus of Example 2 decreases by 2.95Gpa, and the elastic modulus of the cement stone is significantly reduced. When the stratum slips, the crushing of the glass beads (the crushing rate is 96.6%) can provide a larger deformation space, thereby providing a certain buffer space for the deformation of the casing.
  • Example 3 Compared with Comparative Example 3, after adding toughening material and replacing glass beads with a compressive strength of 4000pasi in Example 3, the conventional properties of the cement slurry such as API water loss, fluidity, and compressive strength of the two do not change much, and both meet the construction requirements; however, the elastic modulus of Example 2 decreases by 2.91Gpa, and the elastic modulus of the cement stone is significantly reduced. When the stratum slips, the crushing of the glass beads (the crushing rate is 95.1%) can provide a larger deformation space, thereby providing a certain buffer space for the deformation of the casing.
  • the cement slurry system for relieving casing deformation provided by the present invention has a density of 1.30-1.60 g/cm 3 , an applicable temperature range of 30-150° C., a 7-day cement stone compressive strength of more than 20 MPa, an elastic modulus of less than 5 GPa, and good settlement stability and rheological properties, meeting cementing construction requirements.

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Abstract

本发明提供了一种缓解套管变形的水泥浆体系及其制备方法和应用，该水泥浆体系的原料包括G级油井水泥和其它以G级油井水泥质量为基准的如下百分比的原料：微硅3-6％，玻璃微珠15-50％，增强材料3-6％，增韧材料3-5％，稳定剂0-2％，分散剂0-2.5％，降失水剂3-6％，缓凝剂0-2.5％，消泡剂0.2-0.5％，抑泡剂0.2-0.5％，水70-95％；增韧材料由质量比为2-4:1的纤维和碳材料复配而成，玻璃微珠的抗压强度为3000-5000psi。本发明水泥浆体系的预防、缓解套管变形的效果良好。

Description

一种缓解套管变形的水泥浆体系及其制备方法和应用
交叉引用信息
本申请要求于2023年06月30日提交中国专利局、申请号为202310795333.7、发明名称为“一种套变缓解水泥浆体系及其制备方法和应用”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及页岩气固井技术领域，具体涉及一种缓解套管变形的水泥浆体系及其制备方法和应用。
背景技术
目前，针对页岩气井固井防套管变形(套变)问题普遍采用增大水泥环厚度或者套管壁厚、降低水泥石弹性模量等方法，缓解套变现象，无专门用于页岩气井防套变的固井水泥浆体系。
CN202210052442.5公开了一种页岩气固井用高密度防窜韧性水泥浆体系及其制备方法和应用，其包括G级水泥、水、复合加重剂、纳米防窜剂、增韧剂、降失水剂、缓凝剂、分散剂和消泡剂，其中，纳米防窜剂的加入不仅对水泥浆的施工性能无负面影响，且能够促进水泥早期强度的形成，降低水泥石渗透率，使水泥石的结构变的更加均匀密实，有效的增强水泥石的防窜性。
CN201910113067.9公开了一种适合页岩气水平井大型分段压裂用的固井水泥浆体系，主要包括油井水泥100份、淡水43-46份、弹韧剂2-4份、防窜剂1-2份、降失水剂1-3份、分散剂0.4-0.6份、膨胀剂1-1.5份、缓凝剂0.5-2.0份、消泡剂0.1-0.5份，所述弹韧剂为比表面积≥7m/g，体积压缩率≥5％的橡胶纤维或所述橡胶纤维与橡胶颗粒的混合物。该技术的固井水泥浆体系的稠化防窜性能，弹韧性等综合性能优异可在水泥环承受分段压裂交变载荷作用下有效实现水泥环与套管的同步变形，保证页岩气水平井在后期储层改造和试气生产作业过程中的井筒密封长期完整性，有效预防套管环空带压现象的出现，为页岩气水平井长期生产和大规模压裂提供有效保证。
CN201410471036.8公开了一种水泥用增韧防窜剂及页岩气水平井固井用增韧水泥，该技术涉及一种页岩气水平井固井时使用的水泥浆及其中添加的增韧添加剂，该水泥用增韧防窜剂，由丁苯橡胶粉和可再分散的胶乳粉以2:1的质量比混合而成，其中所述的 丁苯橡胶粉使用前进行了下述处理：先配制质量百分含量为1.5％的硅烷偶联剂溶液，向其中加入丁苯橡胶粉，静置24小时后过滤，晒干制成水泥浆后体系性能稳定，稠化时间易调，失水小于30ml，45度倾角游离液和上下密度差均为0.50℃抗压强度24h大于30Mpa，适用温度范围50-120℃，稠化时间110-240min；所述的页岩气水平井固井用增韧水泥添加了上述水泥用增韧防窜剂。其制成的水泥浆体系稳定性好，失水析水低，能够满足页岩气水平井多级压裂对水泥浆体系的要求。
上述现有技术，在防套变方面取得了成果，但在复杂的套变工况下仍不具备普适性。为此，亟需开展页岩气缓解套变固井水泥浆研究，提升页岩气井固井质量、保障套管服役安全、保障页岩气高效开发。
发明内容
为解决上述技术问题，本发明提供一种缓解套管变形的水泥浆体系及其制备方法，该水泥浆体系成品低、易制得。
为达到上述目的，本发明提供一种缓解套管变形的水泥浆体系，其原料包括G级油井水泥和其它以G级油井水泥质量为基准的如下百分比的原料：微硅3-6％，玻璃微珠15-50％，增强材料3-6％，增韧材料3-5％，稳定剂0-2％，分散剂0-2.5％，降失水剂3-6％，缓凝剂0-2.5％，消泡剂0.2-0.5％，抑泡剂0.2-0.5％，水70-95％；
其中，所述增韧材料由质量比为2-4:1的纤维和碳材料复配而成，所述纤维包括玄武岩纤维、氧化铝纤维、碳化硅纤维中的一种或两种以上的组合，所述碳材料包括碳纳米管和/或膨胀石墨；
所述玻璃微珠的抗压强度为3000-5000psi。
根据本发明的具体实施方案，优选地，以质量份数计，所述缓解套管变形的水泥浆体系的原料包括：G级油井水泥100份，微硅3-6份，玻璃微珠15-50份，增强材料3-6份，增韧材料3-5份，稳定剂0-2份，分散剂0-2.5份，降失水剂3-6份，缓凝剂0-2.5份，消泡剂0.2-0.5份，抑泡剂0.2-0.5份，水70-95份；
其中，所述增韧材料由质量比为2-4:1的纤维和碳材料复配而成，所述纤维包括玄武岩纤维、氧化铝纤维、碳化硅纤维中的一种或两种以上的组合，所述碳材料包括碳纳米管和/或膨胀石墨；所述玻璃微珠的抗压强度为3000-5000psi。
上述缓解套管变形的水泥浆体系中，优选地，所述玻璃微珠的抗压强度为4000psi。
本发明通过添加抗压强度较低的玻璃微珠和由纤维、碳材料复配而成的增韧材料，在不影响水泥石抗压强度的情况下降低其弹性模量，水泥石抗压达到自身抗压能力极限 发生破坏前内部玻璃微珠已破碎，为套管变形提供一定缓冲空间，使水泥石缓解套管变形能力也逐步增强。
上述缓解套管变形的水泥浆体系中，优选地，所述玄武岩纤维的纤维长度为1.5-10μm。
上述缓解套管变形的水泥浆体系中，优选地，所述氧化铝纤维的纤维长度为3-6μm。
上述缓解套管变形的水泥浆体系中，优选地，所述碳化硅纤维的纤维长度为10-15μm。
上述缓解套管变形的水泥浆体系中，优选地，所述碳纳米管的长度为10-30μm。
上述缓解套管变形的水泥浆体系中，优选地，所述膨胀石墨的粒径为40-50μm。
上述缓解套管变形的水泥浆体系中，优选地，所述微硅的平均粒径为4-10μm，45μm筛余≤5％。
上述缓解套管变形的水泥浆体系中，优选地，所述玻璃微珠的真密度为0.38-0.42g/cm3，更优选为0.40g/cm3。本发明优选了玻璃微珠的真密度，玻璃微珠的真密度过大时，破碎后能提供的空间有限。
上述缓解套管变形的水泥浆体系中，优选地，所述稳定剂为矿石粉类稳定剂和/或聚合物类稳定剂，更优选为矿石粉类稳定剂。
上述缓解套管变形的水泥浆体系中，优选地，所述分散剂为甲醛和丙酮的缩聚物和/或聚苯乙烯磺酸盐类分散剂。
上述缓解套管变形的水泥浆体系中，优选地，所述降失水剂为聚丙烯酰胺类降失水剂。
上述缓解套管变形的水泥浆体系中，优选地，所述缓凝剂为丙烯酰胺类缓凝剂。
上述缓解套管变形的水泥浆体系中，优选地，所述消泡剂包括磷酸三丁酯、聚氧丙烯甘油、聚二甲基硅氧烷中的一种或两种以上的组合。
根据本发明的具体实施方案，优选地，所述缓解套管变形的水泥浆体系形成的水泥石的7天抗压强度＞20MPa，弹性模量＜5GPa。
根据本发明的具体实施方案，优选地，所述缓解套管变形的水泥浆体系的密度为1.30-1.60g/cm3，适用温度范围为30-150℃。
本发明还提供一种上述缓解套管变形的水泥浆体系的制备方法，该方法包括：按比例称取原料后混合，在11500-12500r/min转速下搅拌均匀，得到所述缓解套管变形的水泥浆体系。
根据本发明的具体实施方案，优选地，所述缓解套管变形的水泥浆体系的制备方法包括如下步骤：
按比例称取油井水泥、微硅、玻璃微珠、增强材料、增韧材料、稳定剂、分散剂，均匀掺混，得到干混材料；
按比例称取降失水剂、缓凝剂、消泡剂并在水中搅拌均匀，得到湿混药水；
在3800-4200r/min的转速下，将干混料均匀倒入湿混药水中，待干混料完全加入到湿混药水中之后，将搅拌器转速调整至11500-12500r/min，继续搅拌，得到所述缓解套管变形的水泥浆体系。
本发明还提供一种上述缓解套管变形的水泥浆体系在页岩气井固井、防止和/或缓解套管变形中的应用。
本发明提供的技术方案，具有如下有益效果：
本发明提供的缓解套管变形的水泥浆体系了满足固井施工要求，同时水泥石弹性模量较低，地层滑移量较大时还可主动破碎换取空间，为套管变形提供空间，预防和缓解套管变形的效果良好。在一些具体实施方式中，本发明的缓解套管变形的水泥浆体系形成的水泥石的7天抗压强度＞20MPa，弹性模量＜5GPa。
具体实施方式
为了对本发明的技术特征、目的和有益效果有更加清楚的理解，现对本发明的技术方案进行以下详细说明，但不能理解为对本发明的可实施范围的限定。
本发明实施例所用原料说明：
G级油井水泥为高抗硫酸盐型(HSR)G级油井水泥，由大连水泥集团有限公司生产；
稳定剂为中国石油集团工程技术研究院有限公司生产的成熟产品，商品名为“固井油井水泥用增强材料矿石粉类DRB-1S”。
玄武岩纤维为市售，纤维长度为1.5-10μm；
氧化铝纤维为市售，纤维长度为3-6μm；
碳化硅纤维长度为10-15μm；
碳纳米管，纯度95％，长度为10-30μm；
膨胀石墨为市售，纯度95％以上，粒径为48μm(目数300目)；
微硅为市售，平均粒径为5μm，45μm筛余≤5％；
分散剂为甲醛和丙酮的缩聚物或者聚苯乙烯磺酸盐类分散剂中的一种；
降失水剂为聚丙烯酰胺类中的一种；
消泡剂为本领域常用的磷酸三丁酯、聚氧丙烯甘油、聚二甲基硅氧烷中的一种。
实施例1
本实施例提供一种缓解套管变形的水泥浆体系，其制备方法如下：
一、配方
按重量百分比计，该水泥浆配方如下：100份G级油井水泥、5份微硅、10份增强材料、4份增韧材料、13份玻璃微珠、1份稳定剂、1.5份分散剂、3.5份降失水剂、0.8份缓凝剂、0.5份消泡剂、0.5份抑泡剂、70份水；其中，所述增韧材料由2份玄武岩纤维和1份膨胀石墨均匀搅拌而成；玻璃微珠的真密度为0.40g/cm3，抗压强度为4000psi。
二、制备方法
按比例称取油井水泥、微硅、玻璃微珠、增强材料、增韧材料、稳定剂、分散剂并均匀掺混得到干混材料，按比例称取降失水剂、缓凝剂、消泡剂并在水中搅拌均匀得到湿混药水；在4000r/min的转速下，将干混料均匀倒入湿混药水中，待干混料完全加入到湿混药水中之后，盖上搅拌杯杯盖，将搅拌器转速调整至12000r/min，继续搅拌35s，得到缓解套管变形的水泥浆体系。经测试，该水泥浆密度为1.6g/cm3。
实施例2
本实施例提供一种缓解套管变形的水泥浆体系，其制备方法如下：
一、配方
按重量百分比计，该水泥浆配方如下：100份G级油井水泥、5份微硅、10份增强材料、4份增韧材料、32份玻璃微珠、1份稳定剂、1.5份分散剂、3.5份降失水剂、0.8份缓凝剂、0.5份消泡剂、0.5份抑泡剂、75份水；其中，所述增韧材料由3份碳化硅纤维和1份膨胀石墨均匀搅拌而成；所述玻璃微珠的真密度为0.40g/cm3，抗压强度为4000psi。
二、制备方法同实施例1。该水泥浆密度为1.45g/cm3。
实施例3
本实施例提供一种缓解套管变形的水泥浆体系，其制备方法如下：
一、配方
按重量百分比计，该水泥浆配方如下：100份G级油井水泥、5份微硅、10份增强材料、4份增韧材料、50份玻璃微珠、1份稳定剂、1.5份分散剂、3.5份降失水剂、0.8份缓凝剂、0.5份消泡剂、0.5份抑泡剂、78份水；其中，所述增韧材料由4份氧化铝纤维、1份碳纳米管均匀搅拌而成；所述玻璃微珠的真密度为0.40g/cm3，抗压强度为4000psi。
二、制备方法同实施例1。该水泥浆密度为1.3g/cm3。
对比例1
本对比例提供一种水泥浆体系，其配方和制备方法与实施例1相同，区别仅在于，本对比例未添加增韧材料，使用的玻璃微珠的真密度为0.63g/cm3，抗压强度为15000psi；同时，为保持水泥浆密度不变，将水的重量份数更改为68份。
对比例2
本对比例提供一种水泥浆体系，其配方和制备方法与实施例2相同，区别仅在于，本对比例未添加增韧材料，并且玻璃微珠的真密度为0.60g/cm3，抗压强度为12000psi；同时，为保持水泥浆密度不变，将水的重量份数更改为73份。
对比例3
本对比例提供一种水泥浆体系，其配方和制备方法与实施例3相同，区别仅在于，本对比例未添加增韧材料，并且玻璃微珠的真密度为0.60g/cm3，抗压强度为12000psi；同时，为保持水泥浆密度不变，将水的重量份数更改为76份。
实验例
按照国家标准GB/T 19139-2012《油井水泥试验方法》开展实验，对水泥浆体系的常规工程性能(密度、流动度、API失水量)以及抗压强度和弹性模量进行评价。
主要实验仪器有：30-60型瓦棱搅拌器；TG7370D型增压养护釜，沈阳泰格石油仪器设备制造有限公司；HH-420型恒温数显水箱，常州市亿能实验仪器厂；YAW-300B液压式压力试验机，济南新试金试验机有限公司。
本实验例还采用以下方法在规定条件下测试玻璃微珠的破碎率：
1、测量原理
根据样品在规定的压力下，压前密度与压后密度的变化来测定破碎率。
2、仪器设备
强度测试仪、氮气(纯度99.9％)、分析天平。
3、实验步骤
(1)首先取(2-5)g的样品进行真密度测量，仪器采用贝士德仪器科技(北京)有限公司生产的3H-2000TD2型真密度测量仪(或选用其他具备同样真密度测量的仪器)进行测量；
(2)领取同批次(2-5)g放入样品室中，将样品室放进高压仓，锁紧高压仓螺栓；
(3)打开氮气阀，充入氮气，使氮气压力达到所需的压力下，恒压5min，卸去压力，取出样品后进行真密度测量，仪器采用贝士德仪器科技(北京)有限公司生产的3H-2000TD2型真密度测量仪(或选用其他具备同样真密度测量的仪器)进行测量。
4、破碎率计算
压前与压后的样品密度测试根据如下公式计算：
R＝ρ0×(ρ2-ρ2)/ρ2/(ρ0-ρ1)×100
式中：
R—规定条件下的破碎率，％；
ρ0—样品完全破碎下的真密度，g/cm3；
ρ1—样品的压前密度，g/cm3；
ρ2—样品的压后密度，g/cm3。
上述实施例和对比例的水泥浆体系的测试结果如表1所示。
表1水泥浆体系性能测试结果
由表1数据可知，实施例1-3的水泥浆体系流动度均大于20cm，API失水量小于50mL，满足固井施工要求；实施例1-3的水泥浆体系形成的水泥石的7天抗压强度大于20MPa，弹性模量小于5GPa，性能良好，满足固井密封要求。
由对比例1-3的测试结果可知，不加入增韧材料，形成的水泥石抗压强度大于20MPa，但7天弹性模量较高，地层滑移时水泥石变性能力差，易导致应力集中；另外，当地层应力达到水泥石抗压强度极限时水泥石发生破裂，此时内部高抗压玻璃微珠结构基本完好，不能为套变变形提供空间。
比较对比例1和实施例1的结果可知，二者的水泥浆API失水量、流动度、抗压强度等常规性能变化不大，均满足施工要求。与对比例1相比，实施例1添加增韧材料且更换抗压强度为4000pasi的玻璃微珠后，形成的水泥石的弹性模量由7.94GPa下降至4.92GPa，水泥石脆性明显下降，水泥石抗压达到自身抗压能力极限发生破坏前，内部 玻璃微珠已破碎(破碎率为95.1％)，提供的变形空间较大，可为套管变形提供一定缓冲空间。
与对比例2相比，实施例2添加增韧材料且更换抗压强度为4000pasi的玻璃微珠后，二者的水泥浆API失水量、流动度、抗压强度等常规性能变化不大，均满足施工要求；但是，实施例2的弹性模量下降了2.95Gpa，水泥石弹性模量显著降低，当地层产生滑移时，玻璃微珠破碎(破碎率为96.6％)可提供较大的变形空间，从而为套管变形提供一定缓冲空间。
与对比例3相比，实施例3添加增韧材料且更换抗压强度为4000pasi的玻璃微珠后，二者的水泥浆API失水量、流动度、抗压强度等常规性能变化不大，均满足施工要求；但是，实施例2的弹性模量下降了2.91Gpa，水泥石弹性模量显著降低，当地层产生滑移时，玻璃微珠破碎(破碎率为95.1％)可提供较大的变形空间，从而为套管变形提供一定缓冲空间。
综上，本发明提供的缓解套管变形的水泥浆体系，其密度1.30-1.60g/cm3，适用温度范围30-150℃，7天水泥石抗压强度大于20MPa，弹性模量小于5GPa，同时沉降稳定性、流变性良好，满足固井施工要求。
以上所述实施例仅为表达本发明的实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形、同等替换、改进等，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (18)

  1. 一种缓解套管变形的水泥浆体系，其原料包括G级油井水泥和其它以G级油井水泥质量为基准的如下百分比的原料：微硅3-6％，玻璃微珠15-50％，增强材料3-6％，增韧材料3-5％，稳定剂0-2％，分散剂0-2.5％，降失水剂3-6％，缓凝剂0-2.5％，消泡剂0.2-0.5％，抑泡剂0.2-0.5％，水70-95％；
    其中，所述增韧材料由质量比为2-4:1的纤维和碳材料复配而成，所述纤维包括玄武岩纤维、氧化铝纤维、碳化硅纤维中的一种或两种以上的组合，所述碳材料包括碳纳米管和/或膨胀石墨；
    所述玻璃微珠的抗压强度为3000-5000psi。
  2. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述玄武岩纤维的纤维长度为1.5-10μm。
  3. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述氧化铝纤维的纤维长度为3-6μm。
  4. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述碳化硅纤维的纤维长度为10-15μm。
  5. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述碳纳米管的长度为10-30μm。
  6. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述膨胀石墨的粒径为40-50μm。
  7. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述玻璃微珠的真密度为0.38-0.42g/cm3。
  8. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述微硅的平均粒径为4-10μm，45μm筛余≤5％。
  9. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述稳定剂为矿石粉类稳定剂和/或聚合物类稳定剂。
  10. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述分散剂为甲醛和丙酮的缩聚物和/或聚苯乙烯磺酸盐类分散剂。
  11. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述降失水剂为聚丙烯酰胺类降失水剂。
  12. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述缓凝剂为丙烯酰胺类缓凝剂。
  13. 根据权利要求1所述的缓解套管变形的水泥浆体系，其中，所述消泡剂包括磷酸三丁酯、聚氧丙烯甘油、聚二甲基硅氧烷中的一种或两种以上的组合。
  14. 根据权利要求1-13任一项所述的缓解套管变形的水泥浆体系，其中，所述缓解套管变形的水泥浆体系形成的水泥石的7天抗压强度＞20MPa，弹性模量＜5GPa。
  15. 根据权利要求14所述的缓解套管变形的水泥浆体系，其中，所述缓解套管变形的水泥浆体系的密度为1.30-1.60g/cm3，适用温度范围为30-150℃。
  16. 一种权利要求1-15任一项所述的缓解套管变形的水泥浆体系的制备方法，其包括：按比例称取原料后混合，在11500-12500r/min转速下搅拌均匀，得到所述缓解套管变形的水泥浆体系。
  17. 根据权利要求16所述的缓解套管变形的水泥浆体系的制备方法，其中，包括如下步骤：
    按比例称取油井水泥、微硅、玻璃微珠、增强材料、增韧材料、稳定剂、分散剂，均匀掺混，得到干混材料；
    按比例称取降失水剂、缓凝剂、消泡剂并在水中搅拌均匀，得到湿混药水；
    在3800-4200r/min的转速下，将干混料均匀倒入湿混药水中，待干混料完全加入到湿混药水中之后，将搅拌器转速调整至11500-12500r/min，继续搅拌，得到所述缓解套管变形的水泥浆体系。
  18. 权利要求1-15任一项所述的缓解套管变形的水泥浆体系在页岩气井固井、防止和/或缓解套管变形中的应用。
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