CN115716730B - Elastic and tough micro-expansion cement paste and preparation method thereof - Google Patents
Elastic and tough micro-expansion cement paste and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of well cementation cement paste, in particular to elastic and tough micro-expansion cement paste and a preparation method thereof, wherein the raw materials comprise cement, elastic granular materials, coarse silica sand, micro-silica powder, superfine cement, an expanding agent, iron ore powder, a composite fiber toughening agent, a fluid loss agent, a drag reducer, a retarder, a reinforcing agent, a defoaming agent and water, and the preparation method comprises the following steps: mixing cement, elastic granular material, coarse silica sand, silica fume, superfine cement, expanding agent and iron ore powder to obtain solid mixture, adding filtrate reducer, reinforcing agent, drag reducer, retarder and defoaming agent into water, mixing to obtain liquid mixture, mixing the solid mixture and the liquid mixture, adding composite fiber toughening agent, and mixing to obtain the final product. The elastic and ductile micro-expansion cement paste has the characteristics of high compression strength, high tensile strength, low Young modulus, micro-expansion, strong cementing capacity and low permeability, and can meet the trial production requirements of perforation and large-scale fracturing.
Description
Technical Field
The invention relates to the technical field of well cementation cement paste, in particular to elastic and tough micro-expansion cement paste and a preparation method thereof.
Background
The economic and effective development of shale oil can ensure national energy safety and realize the break-through of high-quality development of oil fields. Shale oil is typically developed in a manner that is primarily "horizontal well + volumetric fracturing". The conventional cement stone has large brittleness and volume shrinkage, the elastic modulus of the cement sheath and the elastic modulus of the sleeve are large, obvious crushing phenomenon can be formed under the action of high-energy flow-gathering impact force of the perforating charges, and subsequent fracturing yield-increasing measures can further expand the cracks and even cause complete failure of the sealing function of the cement sheath. Therefore, improving the sealing integrity of the cement sheath becomes a key for efficient development of shale oil horizontal wells.
The shale oil long horizontal well cementing slurry technology currently mainly has two technical schemes. Firstly, the cement paste prepared by adding the rubber powder, the modified rubber powder, the sintered epoxy resin powder, the polytetrafluoroethylene rubber powder and other domestic elastic materials into the conventional cement paste has low temperature resistance, and the rubber powder can erode or has limited Young modulus reduction or complex construction process and limited implementation effect when being contacted with oil. Secondly, the imported elastic material is added into the conventional cement slurry in the middle year, so that the cementing quality and the later development requirement can be guaranteed, but the price is very expensive, the time span of the introduction process is long, the time and the labor are wasted, and the efficient, economical and large-scale development of the shale oil horizontal well is not facilitated.
Disclosure of Invention
The invention provides elastic and tough micro-expansion cement paste and a preparation method thereof, which overcome the defects of the prior art, and can effectively solve the problems of volume shrinkage, poor cementing quality and micro-annular gap generation caused by inconsistent deformation of cement paste and a sleeve under the alternating stress load of temperature and pressure of the conventional cement paste.
One of the technical schemes of the invention is realized by the following measures: the elastic and ductile micro-expansion cement slurry comprises, by weight, 100 parts of cement, 6 to 18 parts of elastic granular materials, 10 to 35 parts of coarse silica sand, 4 to 12 parts of micro silicon powder, 3 to 12 parts of superfine cement, 3 to 6 parts of expansion agent, 0 to 72 parts of iron ore powder, 1 to 2 parts of composite fiber toughening agent, 4 to 5 parts of fluid loss agent, 1 to 2 parts of drag reducer, 0.5 to 4.0 parts of retarder, 0.5 to 2.0 parts of reinforcing agent, 0.5 to 47 parts of defoamer and water.
The following are further optimizations and/or improvements to one of the above-described inventive solutions:
the elastic granular material is hydrogenated nitrile rubber.
The composite fiber toughening agent is a composite fiber material, and the composite fiber material is formed by mixing 40-55% of glass fiber, 40-45% of carbon fiber and the balance of aramid fiber, wherein the glass fiber length is 4-8 mm, the aramid fiber length is 1.5-3.0 mm, and the carbon fiber length is 0.4-1.2 mm.
The said expanding agent is oil well cement expanding agent, which is calcium magnesium oxide (SUP).
The water loss reducing agent is a terpolymer water loss reducing agent, and the terpolymer water loss reducing agent is 2-acrylamide-2-methylpropanesulfonic Acid (AMPS).
The drag reducer is methyl naphthalene sulfonate formaldehyde condensate, and the retarder is sodium gluconate cellulose compound (HS-R).
The reinforcing agent is a mixture of ammonium formate and sodium silicate, the defoaming agent is polyether polyol, the iron ore powder is magnetite powder, and the density is 5.05g/cm 3 。
The grain size of the coarse silica sand is 520-600 mu m, the grain size of the micro silica powder is 0.17-0.28 mu m, and the SiO in the coarse silica sand and the micro silica powder 2 The content is 95-98%, the maximum grain diameter of the superfine cement is not more than 17 mu m, and the grain diameter of more than 80% of grains is below 5 mu m.
The second technical scheme of the invention is realized by the following measures: the preparation method of the elastic and ductile micro-expansion cement paste is carried out according to the following steps: the method comprises the following steps of firstly, fully mixing and uniformly stirring required amounts of cement, elastic particle materials, coarse silica sand, silica fume, superfine cement, an expanding agent and iron ore powder to obtain a solid mixture; secondly, adding a fluid loss agent, an enhancer, a drag reducer, a retarder and a defoamer into required amount of water under the stirring condition, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2-3 min, and the stirring speed is 4000rpm +/-200 rpm; and thirdly, mixing and stirring the solid mixture and the liquid mixture, and then adding the required amount of the composite fiber toughening agent to mix and stir to obtain the elastic micro-expansion cement paste, wherein the stirring time is 30-40 s, and the stirring speed is 4000rpm +/-200 rpm.
The elastic and tough micro-expansion cement paste has the beneficial effects that:
the invention relates to the technical index of elastic and tough micro-expansion cement paste: (1) The density range is 1.70g/cm 3 To 2.20g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the (2) temperature resistance reaches 130 ℃; (3) the free liquid is 0; (4) API water loss<50mL; (5) Compressive strength for 24 hours>14MPa;7d compressive Strength>28MPa; (6) 7d Young's modulus<5000MPa; (7) 7d tensile Strength>2.4MPa (highest requirement of cementing toughness cement technical specification)>1.90 MPa); (8) 24h cement linear expansion coefficient>0.3 percent (highest requirement of cementing toughness cement technical specification)>0.2%); (9) 7d set cement infiltration<0.04x10 -3 μm 2 (highest requirements of well cementation toughness cement technical Specification<0.05x10 -3 μm 2 )。
The elastic and ductile micro-expansion cement paste is introduced into domestic elastic granular material hydrogenated nitrile rubber particles, so that the Young modulus of cement paste can be greatly reduced, the radial deformation capacity of a cement ring is enhanced, the cement paste and a sleeve can be synchronously deformed, micro-cracks and micro-annular gaps are avoided, and the cost of raw materials is relatively low.
The elastic and ductile micro-expansion cement slurry provided by the invention introduces the composite fiber toughening agent, realizes the mutual synergistic effect of long and short fibers, overcomes the defect that the single use of long fibers is easy to agglomerate when being applied on site, and overcomes the defects of short fiber lacing bridging and weak impact resistance, so that the cement stone has stronger impact resistance, higher flexural strength and greatly improved cementing strength, and simultaneously has the functions of leakage prevention and plugging.
The elastic and ductile micro-expansion cement slurry provided by the invention introduces superfine cement, obviously reduces the permeability of the cement stone, and greatly improves the compressive strength and the cementing capacity of the cement stone.
The elastic and ductile micro-expansion cement slurry provided by the invention is introduced with the expanding agent, so that the formation of ettringite in early stage of cement hydration can be promoted, the micro volume expansion is generated, the volume shrinkage in the cement hydration process can be compensated, the cement stone two-interface cementing strength is improved, and the generation of micro annular gaps is avoided.
According to the invention, the fluid loss agent, the retarder and the drag reducer are introduced into the liquid mixture, and the reinforcing agent which is easy to dissolve in water is added to form a synergistic effect, so that the flexible micro-expansion cement slurry has the advantages of good rheological property, low water loss, zero water evolution, stable slurry, adjustable thickening time, short thickening test transition time and outstanding channeling prevention effect.
The invention breaks through the limitations of volume shrinkage, poor cementing quality and micro annular gap generated by inconsistent deformation of the cement stone and the sleeve under the alternating stress load of temperature and pressure of the conventional cement stone, the invention carries out mechanical property modification on the conventional cement stone, and the obtained low-density and high-density cement paste both meets the requirements of lower Young modulus of the cement stone, higher compressive strength and tensile strength, can resist external force deformation, has low permeability and micro expansion of the cement stone, and meets the requirements of perforation and large-scale fracturing exploitation.
In a word, the elastic and ductile micro-expansion cement paste has the characteristics of high compression strength, high tensile strength, low Young modulus, micro-expansion, strong cementing capacity and low permeability, can meet the test production requirements of perforation and large-scale fracturing, and has good cement sheath integrity after fracturing.
Drawings
FIG. 1 is a thickening graph of a flexible micro-expansive cement slurry of the present invention.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention. The various chemical reagents and chemical supplies mentioned in the invention are all commonly known and used in the prior art unless specified otherwise; the percentages in the invention are mass percentages unless otherwise specified.
The invention is further described below with reference to examples:
example 1: the elastic and ductile micro-expansion cement slurry comprises, by weight, 100 parts of cement, 6 to 18 parts of elastic granular materials, 10 to 35 parts of coarse silica sand, 4 to 12 parts of micro silicon powder, 3 to 12 parts of superfine cement, 3 to 6 parts of expansion agent, 0 to 72 parts of iron ore powder, 1 to 2 parts of composite fiber toughening agent, 4 to 5 parts of fluid loss additive, 1 to 2 parts of drag reducer, 0.5 to 4.0 parts of retarder, 0.5 to 2.0 parts of reinforcing agent, 0.5 to 47 parts of defoamer and 57 parts of water.
The elastic granular material is hydrogenated nitrile rubber. The hydrogenated nitrile rubber is a hydrogenation product of butadiene-acrylonitrile copolymer, and has good heat resistance, oil resistance and chemical corrosion resistance.
The composite fiber toughening agent is a composite fiber material, and the composite fiber material is formed by mixing 40-55% of glass fiber, 40-45% of carbon fiber and the balance of aramid fiber, wherein the glass fiber length is 4-8 mm, the aramid fiber length is 1.5-3.0 mm, and the carbon fiber length is 0.4-1.2 mm.
The said expanding agent is oil well cement expanding agent, which is calcium magnesium oxide (SUP).
The water loss reducing agent is a terpolymer water loss reducing agent, and the terpolymer water loss reducing agent is 2-acrylamide-2-methylpropanesulfonic Acid (AMPS). AMPS is a terpolymer of Acrylamide (AM) and N-vinyl pyrrolidone (NVP), has an average molecular weight of 68 ten thousand, a short and moderate molecular chain length, and strong temperature resistance, and the temperature resistance can reach 160 ℃.
The drag reducer is methyl naphthalene sulfonate formaldehyde condensate, and the retarder is sodium gluconate cellulose compound (HS-R). The retarder is insensitive to temperature and doping amount, has good retarding effect, and can develop the strength of the cement stone faster.
The reinforcing agent is a mixture of ammonium formate and sodium silicate, the defoaming agent is polyether polyol, the iron ore powder is magnetite powder, and the density is 5.05g/cm 3 . The reinforcing agent is easy to dissolve in water, can obviously shorten the transition time of cement paste thickening experiments, improves the early strength of cement stones, and has less influence on the rheological property of cement paste.
The grain size of the coarse silica sand is 520-600 mu m, the grain size of the micro silica powder is 0.17-0.28 mu m, and the SiO in the coarse silica sand and the micro silica powder 2 The content is 95-98%, the maximum grain diameter of the superfine cement is not more than 17 mu m, and the grain diameter of more than 80% of grains is below 5 mu m.
The elastic and ductile micro-expansion cement paste is prepared by the following steps: the method comprises the following steps of firstly, fully mixing and uniformly stirring required amounts of cement, elastic particle materials, coarse silica sand, silica fume, superfine cement, an expanding agent and iron ore powder to obtain a solid mixture; secondly, adding a fluid loss agent, an enhancer, a drag reducer, a retarder and a defoamer into required amount of water under the stirring condition, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2-3 min, and the stirring speed is 4000rpm +/-200 rpm; and thirdly, mixing and stirring the solid mixture and the liquid mixture, and then adding the required amount of the composite fiber toughening agent to mix and stir to obtain the elastic micro-expansion cement paste, wherein the stirring time is 30-40 s, and the stirring speed is 4000rpm +/-200 rpm.
In the present invention, the swelling agent calcium magnesium oxide (SUP) and retarder sodium gluconate cellulose complex (HS-R) are supplied by chengdou river chemical engineering limited.
Example 2: the elastic toughness micro-expansion cement slurry is prepared from 100g of cement, 18g of hydrogenated nitrile rubber, 10g of coarse silica sand, 10g of silica fume, 12g of superfine cement, 6g of calcium magnesium oxide (SUP), 1.5g of composite fiber toughening agent, 5g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 1.3g of sodium methyl naphthalene sulfonate formaldehyde condensate, 0.8g of sodium gluconate cellulose complex (HS-R), 1.0g of mixture of ammonium formate and sodium silicate, 0.5g of polyether polyol and 57g of water by the following steps: the method comprises the steps of firstly, fully mixing and stirring required amounts of cement, hydrogenated nitrile rubber, coarse silica sand, silica fume, superfine cement and calcium magnesium oxide (SUP) uniformly to obtain a solid mixture; secondly, adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), a mixture of ammonium formate and sodium silicate, a sodium methylnaphthalene sulfonate formaldehyde condensate, a sodium gluconate cellulose compound (HS-R) and polyether polyol into required amount of water under the condition of stirring, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2min, and the stirring speed is 3800rpm; thirdly, mixing and stirring the solid mixture and the liquid mixture, then adding the required amount of the composite fiber toughening agent, mixing and stirring to obtain the elastic toughness micro-powderExpanding cement paste, wherein the stirring time is 30s, and the stirring speed is 3800rpm; the composite fiber toughening agent is formed by mixing 40% of glass fiber, 40% of carbon fiber and the balance of aramid fiber, wherein the glass fiber is 4mm in length, the aramid fiber is 1.5mm in length, the carbon fiber is 0.4mm in length, the coarse silica sand is 520 mu m in particle size, the micro silica powder is 0.17 mu m in particle size, and SiO in the coarse silica sand and the micro silica powder is the same as the glass fiber 2 The content is 95%, the maximum grain diameter of the superfine cement is not more than 17 mu m, and the grain diameter of more than 80% of grains is less than 5 mu m.
Example 3: the elastic toughness micro-expansion cement slurry is prepared from 100g of cement, 8g of hydrogenated nitrile rubber, 12g of coarse silica sand, 8g of silica fume, 9g of superfine cement, 4g of calcium magnesium oxide (SUP), 1.5g of composite fiber toughening agent, 5g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 1.3g of sodium methyl naphthalene sulfonate formaldehyde condensate, 0.8g of sodium gluconate cellulose complex (HS-R), 0.8g of mixture of ammonium formate and sodium silicate, 0.5g of polyether polyol and 49g of water by the following steps: the method comprises the steps of firstly, fully mixing and stirring required amounts of cement, hydrogenated nitrile rubber, coarse silica sand, silica fume, superfine cement and calcium magnesium oxide (SUP) uniformly to obtain a solid mixture; secondly, adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), a mixture of ammonium formate and sodium silicate, a sodium methylnaphthalene sulfonate formaldehyde condensate, a sodium gluconate cellulose compound (HS-R) and polyether polyol into required amount of water under the condition of stirring, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 3min, and the stirring speed is 4200rpm; thirdly, mixing and stirring the solid mixture and the liquid mixture, then adding a required amount of composite fiber toughening agent, mixing and stirring to obtain the elastic and tough micro-expansion cement paste, wherein the stirring time is 40s, and the stirring speed is 4200rpm; the composite fiber toughening agent is formed by mixing 55% of glass fiber, 45% of carbon fiber and the balance of aramid fiber, wherein the glass fiber is 8mm in length, the aramid fiber is 3.0mm in length, the carbon fiber is 1.2mm in length, the coarse silica sand is 600 mu m in particle size, the micro silica powder is 0.28 mu m in particle size, and SiO in the coarse silica sand and the micro silica powder is the same as the glass fiber 2 The content of the superfine cement is 98%, the maximum grain diameter of the superfine cement is not more than 17 mu m, and the content of the superfine cement is more than 80%The particle size of the particles is below 5 μm.
Example 4: the elastic toughness micro-expansion cement slurry is prepared from 100g of cement, 7g of hydrogenated nitrile rubber, 10g of coarse silica sand, 4g of silica fume, 6g of superfine cement, 4g of calcium magnesium oxide (SUP), 1.5g of composite fiber toughening agent, 4g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 1.5g of sodium methyl naphthalene sulfonate formaldehyde condensate, 0.8g of sodium gluconate cellulose complex (HS-R), 0.6g of mixture of ammonium formate and sodium silicate, 0.5g of polyether polyol and 47g of water by the following steps: the method comprises the steps of firstly, fully mixing and stirring required amounts of cement, hydrogenated nitrile rubber, coarse silica sand, silica fume, superfine cement and calcium magnesium oxide (SUP) uniformly to obtain a solid mixture; secondly, adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), a mixture of ammonium formate and sodium silicate, a sodium methylnaphthalene sulfonate formaldehyde condensate, a sodium gluconate cellulose compound (HS-R) and polyether polyol into required amount of water under the condition of stirring, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2.5min, and the stirring speed is 4000rpm; thirdly, mixing and stirring the solid mixture and the liquid mixture, then adding a required amount of composite fiber toughening agent, mixing and stirring to obtain the elastic and tough micro-expansion cement paste, wherein the stirring time is 35s, and the stirring speed is 4000rpm; the composite fiber toughening agent is formed by mixing 50% of glass fiber, 42% of carbon fiber and the balance of aramid fiber, wherein the glass fiber is 6mm in length, the aramid fiber is 2.0mm in length, the carbon fiber is 0.8mm in length, the coarse silica sand is 560 mu m in particle size, the micro silica powder is 0.22 mu m in particle size, and SiO in the coarse silica sand and the micro silica powder is formed by mixing 2 The content is 97%, the maximum particle size of the superfine cement is not more than 17 mu m, and the particle size of more than 80% of particles is less than 5 mu m.
Example 5: the elastic toughness micro-expansion cement slurry comprises 100g of cement, 9g of hydrogenated nitrile rubber, 30g of coarse silica sand, 10g of silica fume, 10g of superfine cement, 4g of calcium magnesium oxide (SUP), 44g of magnetite powder, 1g of composite fiber toughening agent, 5g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 1.3g of sodium methyl naphthalene sulfonate formaldehyde condensate, 2g of sodium gluconate cellulose complex (HS-R), ammonium formate and silicic acidA mixture of sodium 0.6g, polyether polyol 0.5g and 49g water was obtained as follows: the first step, fully mixing and stirring required amounts of cement, hydrogenated nitrile rubber, coarse silica sand, silica fume, superfine cement, calcium magnesium oxide (SUP) and magnetite powder uniformly to obtain a solid mixture; secondly, adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), a mixture of ammonium formate and sodium silicate, a sodium methylnaphthalene sulfonate formaldehyde condensate, a sodium gluconate cellulose compound (HS-R) and polyether polyol into required amount of water under the condition of stirring, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2.5min, and the stirring speed is 4000rpm; thirdly, mixing and stirring the solid mixture and the liquid mixture, then adding a required amount of composite fiber toughening agent, mixing and stirring to obtain the elastic and tough micro-expansion cement paste, wherein the stirring time is 35s, and the stirring speed is 4000rpm; the composite fiber toughening agent is formed by mixing 48% of glass fiber, 42% of carbon fiber and the balance of aramid fiber, wherein the glass fiber is 6mm in length, the aramid fiber is 2.0mm in length, the carbon fiber is 0.8mm in length, the coarse silica sand is 560 mu m in particle size, the micro silica powder is 0.22 mu m in particle size, and SiO in the coarse silica sand and the micro silica powder is formed by mixing 2 The content is 97%, the maximum particle size of the superfine cement is not more than 17 mu m, and the particle size of more than 80% of particles is less than 5 mu m.
Example 6: the elastic toughness micro-expansion cement slurry is prepared from 100g of cement, 7g of hydrogenated nitrile rubber, 30g of coarse silica sand, 12g of silica fume, 10g of superfine cement, 4g of calcium magnesium oxide (SUP), 72g of magnetite powder, 1g of composite fiber toughening agent, 5g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 1.3g of sodium methyl naphthalene sulfonate formaldehyde condensate, 2g of sodium gluconate cellulose complex (HS-R), 0.6g of a mixture of ammonium formate and sodium silicate, 0.5g of polyether polyol and 52g of water by the following steps: the first step, fully mixing and stirring required amounts of cement, hydrogenated nitrile rubber, coarse silica sand, silica fume, superfine cement, calcium magnesium oxide (SUP) and magnetite powder uniformly to obtain a solid mixture; second, adding a mixture of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), ammonium formate and sodium silicate to a desired amount of water with stirringFully and uniformly mixing the mixture, methyl naphthalene sulfonate formaldehyde condensate, sodium gluconate cellulose complex (HS-R) and polyether polyol to obtain a liquid mixture, wherein the stirring time is 2.5min, and the stirring speed is 4000rpm; thirdly, mixing and stirring the solid mixture and the liquid mixture, then adding a required amount of composite fiber toughening agent, mixing and stirring to obtain the elastic and tough micro-expansion cement paste, wherein the stirring time is 35s, and the stirring speed is 4000rpm; the composite fiber toughening agent is formed by mixing 48% of glass fiber, 42% of carbon fiber and the balance of aramid fiber, wherein the glass fiber is 6mm in length, the aramid fiber is 2.0mm in length, the carbon fiber is 0.8mm in length, the coarse silica sand is 560 mu m in particle size, the micro silica powder is 0.22 mu m in particle size, and SiO in the coarse silica sand and the micro silica powder is formed by mixing 2 The content is 97%, the maximum particle size of the superfine cement is not more than 17 mu m, and the particle size of more than 80% of particles is less than 5 mu m.
The elastic and ductile micro-expansion cement paste obtained in the examples 2 to 6 has the characteristics of high compressive and tensile strength, low Young's modulus, micro-expansion, strong cementing capacity and low permeability. The following are the temperature resistance test of the raw material fluid loss agent of the present invention and the comprehensive performance test and thickening test of the elastic and ductile micro-expansive cement slurries obtained in examples 2 to 6 of the present invention.
Test 1: the temperature resistance test of the raw material fluid loss agent.
The test method comprises the following steps: the raw material fluid loss agent is added into G-grade cement of a sand bay oil well to prepare cement slurry, and the cement slurry is subjected to a fluid loss test according to a specified method in GB/T19139-2012 oil well cement test method. The cement paste comprises the following formula: 100G of G-stage cement, 3.5G to 5.0G of fluid loss agent (the addition amount of the fluid loss agent is 3.5 to 5.0 percent of the G-stage cement), 0.8G to 1.2G of drag reducer and 42G of tap water.
Test results: as shown in table 1, it is clear from table 1 that the cement slurry obtained when the addition amount of the fluid loss agent is 5.0% of the G-stage cement has a lower water loss amount at 160 ℃, which means that the fluid loss agent of the present invention has a better temperature resistance when the addition amount of the fluid loss agent is 4% to 5% of the cement weight.
Test 2: the invention relates to a comprehensive performance test of elastic and ductile micro-expansion cement paste.
The test method comprises the following steps: the elastic and ductile micro-expansion cement slurries obtained in the examples 2 to 6 of the present invention were examined for comprehensive properties including the density, free fluid, API water loss, rheological properties of the cement slurry and mechanical properties (compressive strength, young's modulus, tensile strength and expansion rate) of hardened set cement, wherein the density, free fluid, API water loss, rheological properties of the cement slurry were carried out with reference to the methods specified in GB/T19139-2012 "oil well cement test method"; the compressive strength of the cement stone is carried out according to the method specified in GB/T19139-2012 oil well Cement test method; young's modulus and tensile strength are measured by a rock triaxial stress meter, expansion rate is measured by a method specified by JC/T313-2009 expansion Cement expansion rate test method, compressive strength, young's modulus, tensile strength and expansion rate of cement stones are all tested after curing at 106 ℃ and 74 MPa.
Test results: as shown in Table 2, it is evident from Table 2 that the density range of the elastic-toughness micro-expansive cement slurries obtained in examples 2 to 6 of the present invention is 1.70g/cm 3 To 2.20g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The free liquid is 0; API water loss<50mL; compressive strength for 24 hours>14MPa;7d compressive Strength>28MPa;7d Young's modulus<5000MPa;7d tensile Strength>2.4MPa (highest requirement of cementing toughness cement technical specification)>1.90 MPa); 24h cement linear expansion coefficient>0.3 percent (highest requirement of cementing toughness cement technical specification)>0.2%). The elastic and ductile micro-expansion cement paste disclosed by the invention has excellent performance, and can meet the test production requirements of perforation and large-scale fracturing.
Test 3: thickening test of the elastic and ductile micro-expansive cement paste.
The test method comprises the following steps: the elastic and ductile micro-expansive cement slurry obtained in the embodiment 6 of the invention is subjected to a thickening test, wherein the thickening test is carried out by referring to a method specified in GB/T19139-2012 oil well cement test method, and the test condition is 123 ℃ x108MPax90min.
Test results: as shown in FIG. 1, FIG. 1 shows that the elastic and tough micro-expansive cement slurry obtained in example 6 of the invention has low initial consistency, adjustable thickening time, short transition time and good channeling prevention effect.
In conclusion, the elastic and ductile micro-expansion cement paste has the characteristics of high compressive strength, high tensile strength, low Young modulus, micro-expansion, strong cementing capacity and low permeability, can meet the test production requirements of perforation and large-scale fracturing, and has good cement sheath integrity after fracturing.
The technical characteristics form the embodiment of the invention, have stronger adaptability and implementation effect, and can increase or decrease unnecessary technical characteristics according to actual needs so as to meet the requirements of different situations.
Claims (4)
1. The elastic and tough micro-expansion cement slurry is characterized by comprising, by weight, 100 parts of cement, 6 to 18 parts of hydrogenated nitrile rubber, 10 to 35 parts of coarse silica sand, 4 to 12 parts of micro silicon powder, 3 to 12 parts of superfine cement, 3 to 6 parts of expansion agent, 0 to 72 parts of iron ore powder, 1 to 2 parts of composite fiber toughening agent, 4 to 5 parts of fluid loss agent, 1 to 2 parts of drag reducer, 0.5 to 4.0 parts of retarder, 0.5 to 2.0 parts of reinforcing agent, 0.5 part of defoamer and 47 to 57 parts of water, wherein the cement slurry is prepared by the following steps: the method comprises the following steps of firstly, fully mixing and uniformly stirring required amounts of cement, hydrogenated nitrile rubber, coarse silica sand, silica fume, superfine cement, an expanding agent and iron ore powder to obtain a solid mixture; wherein the expanding agent is oil well cement expanding agent, the oil well cement expanding agent is calcium magnesium oxide, the maximum grain diameter of the superfine cement is not more than 17 mu m, and the grain diameter of more than 80% of grains is below 5 mu m; secondly, adding a fluid loss agent, an enhancer, a drag reducer, a retarder and a defoamer into required amount of water under the stirring condition, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2-3 min, and the stirring speed is 4000rpm +/-200 rpm; the retarder is a sodium gluconate cellulose compound, the reinforcing agent is a mixture of ammonium formate and sodium silicate, the fluid loss additive is a terpolymer fluid loss additive, and the terpolymer fluid loss additive is 2-acrylamido-2-methylpropanesulfonic acid; thirdly, mixing and stirring the solid mixture and the liquid mixture, then adding a required amount of composite fiber toughening agent, mixing and stirring to obtain the elastic and tough micro-expansion cement paste, wherein the stirring time is 30-40 s, and the stirring speed is 4000rpm +/-200 rpm; the composite fiber toughening agent is a composite fiber material, and the composite fiber material is formed by mixing 40-55% of glass fiber, 40-45% of carbon fiber and the balance of aramid fiber, wherein the glass fiber length is 4-8 mm, the aramid fiber length is 1.5-3.0 mm, and the carbon fiber length is 0.4-1.2 mm.
2. The elastic and ductile micro-expansive cement slurry according to claim 1, characterized in that the drag reducer is methyl naphthalene sulfonate formaldehyde condensate, the defoamer is polyether polyol, the iron ore powder is magnetite powder, and the density is 5.05g/cm 3 。
3. The elastic and ductile micro-expansive cement slurry according to claim 1 or 2, characterized in that the coarse silica sand has a particle size of 520 μm to 600 μm and the micro silica powder has a particle size of 0.17 μm to 0.28 μm, and the SiO in the coarse silica sand and the micro silica powder 2 The content is 95 to 98 percent.
4. A method of preparing a flexible micro-expansive cement slurry according to any of claims 2 to 3, characterized by the following method: the method comprises the following steps of firstly, fully mixing and uniformly stirring required amounts of cement, elastic particle materials, coarse silica sand, silica fume, superfine cement, an expanding agent and iron ore powder to obtain a solid mixture; secondly, adding a fluid loss agent, an enhancer, a drag reducer, a retarder and a defoamer into required amount of water under the stirring condition, and fully and uniformly mixing to obtain a liquid mixture, wherein the stirring time is 2-3 min, and the stirring speed is 4000rpm +/-200 rpm; and thirdly, mixing and stirring the solid mixture and the liquid mixture, and then adding the required amount of the composite fiber toughening agent to mix and stir to obtain the elastic micro-expansion cement paste, wherein the stirring time is 30-40 s, and the stirring speed is 4000rpm +/-200 rpm.
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