CN113072315B - Well cementation cement additive and using method thereof - Google Patents
Well cementation cement additive and using method thereof Download PDFInfo
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- CN113072315B CN113072315B CN202110314339.9A CN202110314339A CN113072315B CN 113072315 B CN113072315 B CN 113072315B CN 202110314339 A CN202110314339 A CN 202110314339A CN 113072315 B CN113072315 B CN 113072315B
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- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- 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
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- 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
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- 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
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention discloses a well cementation cement additive and a use method thereof, wherein the well cementation cement additive comprises the following components in percentage by mass in cement: 2-35% of high-strength hollow glass beads, 1-20% of micro-silicon, 0.02-10% of cross-linked calcium alginate fibers, 0.01-3% of retarder and 0.01-3% of dispersant. The raw materials in the well cementation cement additive are compatible for use, so that the density of a well cementation cement slurry system can be effectively reduced, the cement strength is improved, and the cement additive can be used for well cementation of low-pressure easily-leaked stratums.
Description
Technical Field
The invention relates to the technical field of oil field well cementation. More particularly, the present invention relates to a cement additive for well cementing and a method of using the same.
Background
The oil field well drilling area has the characteristics of low pressure, low permeability, low pressure high permeability, crack development, complex pressure system and the like, the development difficulty is increased day by day, and meanwhile, a low-pressure oil leakage layer is formed due to pressure loss caused by unbalanced extraction and injection or formation pressure driving energy loss. The cement paste column pressure is high, the leakage probability is high during the well cementation construction, the target layer cannot be sealed, and the cement squeezing is needed for remediation. With the further expansion of exploration areas and the increase of the drilling depth of oil wells, the leakage wells at oil layer intervals tend to rise year by year, and the technical problem becomes a bottleneck influencing the well cementation quality. Because the plugging effect is not ideal in the well completion stage, the effective method is to use the low-density cement slurry with the plugging effect, reduce the liquid column pressure during the well cementation construction and prevent the cement slurry from being leaked in the well cementation process. The low-density cement slurry generally has lower compressive strength due to larger water-solid ratio and external admixture, and the environmental protection aspect of the low-density cement slurry needs to be improved.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
It is still another object of the present invention to provide a cement additive for well cementation and a method for using the same, which can be used for well cementation of low pressure and easy-to-leak stratum, and has little harm to the environment and excellent comprehensive performance.
To achieve these objects and other advantages in accordance with the present invention, there is provided a cement additive for well cementation, comprising the following components in percentage by mass in cement: 2-35% of high-strength hollow glass beads, 1-20% of micro-silicon, 0.02-10% of cross-linked calcium alginate fibers, 0.01-3% of retarder and 0.01-3% of dispersant.
Preferably, the preparation method of the cross-linked calcium alginate fiber comprises the following steps:
step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 8-10 to prepare a mixed system;
step two, adding epoxy chloropropane accounting for 3-7% of the mass of the sodium alginate into the mixed system, reacting for 1.5-3.5 h at 40-60 ℃, adding absolute ethyl alcohol, performing suction filtration, and drying to obtain the cross-linked sodium alginate;
dissolving the crosslinked sodium alginate in water, standing and defoaming to prepare a crosslinked sodium alginate solution with the mass percent of 3-5%;
and step four, extruding the cross-linked sodium alginate solution into a calcium chloride solution with the mass percent of 1-5% through a spinneret orifice, controlling the temperature of a coagulating bath to be 40 ℃, and obtaining the cross-linked calcium alginate fiber after traction, water washing and drying.
Preferably, the pH is adjusted to 10 in said step one.
Preferably, the epichlorohydrin accounts for 5% of the mass of the sodium alginate in the second step.
Preferably, the diameter of the cross-linked calcium alginate fiber is 100-600 μm.
Preferably, the average diameter of the high-strength hollow glass beads is 0.2 to 0.3 μm.
Preferably, the average diameter of the microsilica is 0.05 to 0.3 μm.
The invention also provides a using method of the well cementation cement additive, which comprises the following steps:
step one, uniformly mixing cement and water to prepare cement paste;
cutting the cross-linked calcium alginate fibers into short fibers;
taking quarter of cement paste, stirring and dispersing the short fibers, the high-strength hollow glass microspheres, the micro-silicon, the retarder and the dispersing agent into the cement paste, and pre-impregnating by using an ultrasonic impregnation method;
and step four, putting the pre-impregnated mixture into the residual cement slurry for full mixing to prepare the well cementation cement slurry, wherein the mass percentage of each component in the cement is as follows: 2-35% of high-strength hollow glass beads, 1-20% of micro-silicon, 0.02-10% of cross-linked calcium alginate fibers, 0.01-3% of retarder and 0.01-3% of dispersant.
Preferably, the length of the short fiber is 0.1-10 mm.
The invention at least comprises the following beneficial effects:
firstly, the invention utilizes the advantages of the calcium alginate fiber such as hydrophilicity, good biocompatibility, thermal irreversibility and the like, and cross-links the calcium alginate fiber, thereby improving the strength and salt tolerance of the material, the cross-linked calcium alginate fiber has a three-dimensional network structure, restrains more free liquid, prevents free water in cement paste from permeating into a permeable stratum, controls water loss, improves the effects of salt tolerance and water loss reduction, and the calcium alginate is a degradable nontoxic environment-friendly material with little harm to the environment;
secondly, the cement additive for well cementation disclosed by the invention adopts high-strength hollow glass beads as lightening materials, takes microsilica as a filling agent, can effectively control the density of cement slurry by controlling the addition amount of the beads, avoids leaking stratum, and improves the void structure of cement and the strength of the cement slurry as the microspheres, the microsilica, fibers and cement particles form compact accumulation.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples to enable those skilled in the art to practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or combinations thereof.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
The invention provides a well cementation cement additive, which comprises the following components in percentage by mass in cement: 2-35% of high-strength hollow glass beads, 1-20% of micro-silicon, 0.02-10% of cross-linked calcium alginate fibers, 0.01-3% of retarder and 0.01-3% of dispersant. The main component of the high-strength hollow glass bead is soda lime borosilicate glass, the high-strength hollow glass bead is water-insoluble pure white, independent and thin-walled hollow particles, and the density of the high-strength hollow glass bead is 0.45-0.65 g/cm3And the compressive strength can reach 115 MPa. The high-strength hollow glass beads can effectively reduce the density of the well cementation liquid, but the slurry sedimentation stability is poor due to the excessively high content, so that the difference of the upper density and the lower density of a condensate is increased. The microsilica is an ultra-fine spherical particle in which amorphous SiO is present2The content of the calcium carbonate accounts for more than 95 percent, and the calcium carbonate can be reacted with the product Ca (OH) during the hydration reaction of the cement2The reaction produces an aqueous calcium silicate hydrate, which produces a poorly permeable set cement structure. And because the particles of the micro-silicon are very small and have large specific surface area, a large amount of water molecules can be adsorbed around the particles, and the water molecules form a uniform and compact net structure through the action of hydrogen bonds, thereby improving the sedimentation stability of cement paste, and the cement paste is more closely stacked through the reasonable grading with the particles of the high-strength hollow glass microspheres, the cross-linked calcium alginate fibers and the like, thereby further improving the effect of the micro-silicon on the cement pasteThe strength and the anti-permeability of the set cement are improved, and the fluid loss reducing capability of the cement paste is improved. The crosslinked calcium alginate fiber forms non-thermoreversible gel by utilizing sodium alginate and calcium ions, is crosslinked, improves the strength and salt resistance of the fiber, is applied to a well cementation cement additive, can be adsorbed on the surface of cement particles to form an adsorption hydration layer, and enables the cement particles to be bridged to form a net structure, so that more free water is bound, gaps among the cement particles are blocked, the permeability of a cement filter cake is reduced, and the permeability is obviously reduced. The retarder plays a role in prolonging or maintaining the time that the well cementation liquid system is in a liquid state and a pumpable state, so that the well cementation liquid system keeps plasticity for a longer time. The dispersant has the functions of improving the slurry preparation capacity of the cement slurry and enhancing the fluidity of the cement slurry, thereby achieving the purposes of dispersion and drag reduction.
In another technical scheme, the preparation method of the cross-linked calcium alginate fiber comprises the following steps:
step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 8-10 to prepare a mixed system;
step two, adding epoxy chloropropane accounting for 3-7% of the mass of the sodium alginate into the mixed system, reacting for 1.5-3.5 h at 40-60 ℃, adding absolute ethyl alcohol, performing suction filtration, and drying to obtain the cross-linked sodium alginate;
dissolving the crosslinked sodium alginate in water, standing and defoaming to prepare a crosslinked sodium alginate solution with the mass percentage of 3-5%;
extruding the cross-linked sodium alginate solution into 1-5 wt% calcium chloride solution through a spinneret orifice, controlling the temperature of a coagulating bath at 40 ℃, and drawing, washing and drying to obtain the cross-linked calcium alginate fiber.
The technical scheme can also comprise the following technical details so as to better realize the technical effects: the preparation method of the cross-linked calcium alginate fiber comprises the following steps:
step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 8-10 to prepare a mixed system;
step two, adding epoxy chloropropane accounting for 3-7% of the mass of the sodium alginate into the mixed system, reacting for 1.5-3.5 h at 40-60 ℃, adding absolute ethyl alcohol, performing suction filtration, and drying to obtain the cross-linked sodium alginate;
step three, mixing and dissolving crosslinked sodium alginate and sodium carboxymethylcellulose in water according to a molar ratio of 20:3, filtering, standing and defoaming to prepare a mixed spinning solution with the mass percentage of 3% -5%;
and step four, taking a calcium chloride solution with the mass percent of 1-5% as a coagulating bath, extruding the mixed spinning solution into the coagulating bath through a spinneret orifice, wherein the temperature of the coagulating bath is 40 ℃, and then drawing, washing and drying to obtain the cross-linked calcium alginate fiber. In the technical scheme, the sodium carboxymethylcellulose and the sodium alginate have similar macromolecular chain structures and good biocompatibility, and the sodium carboxymethylcellulose and the crosslinked sodium alginate are blended to form an interpenetrating network structure, so that the flexibility of the calcium alginate fiber is increased, and the hygroscopicity is improved.
In another embodiment, the pH is adjusted to 10 in step one.
In another technical scheme, the epichlorohydrin accounts for 5% of the mass of the sodium alginate in the second step.
In another technical scheme, the diameter of the cross-linked calcium alginate fiber is 100-600 μm.
In another technical scheme, the average diameter of the high-strength hollow glass beads is 0.2-0.3 μm.
In another technical scheme, the average diameter of the micro silicon is 0.05-0.3 μm.
The invention also provides a using method of the well cementation cement additive, which comprises the following steps:
step one, mixing cement and water uniformly to prepare cement paste;
cutting the cross-linked calcium alginate fibers into short fibers;
taking one fourth of cement paste, dispersing the short fibers, the high-strength hollow glass beads, the micro-silicon, the retarder and the dispersing agent into the cement paste while stirring, and pre-impregnating by using an ultrasonic impregnation method;
and step four, putting the pre-impregnated mixture into the residual cement slurry for fully mixing to prepare the well cementation cement slurry, wherein the mass percentage of each component in the cement is as follows: 2-35% of high-strength hollow glass beads, 1-20% of micro-silicon, 0.02-10% of cross-linked calcium alginate fibers, 0.01-3% of retarder and 0.01-3% of dispersant. The ultrasonic impregnation technology in the technical scheme is characterized in that the cement impregnation material is changed by utilizing the high temperature, high pressure and local shock wave action generated when bubbles are broken in liquid by ultrasound. The ultrasonic impregnation technology can improve the bonding effect of the cross-linked calcium alginate fibers, the high-strength hollow glass microspheres and the micro-silicon particles with the cement surface, and improve the interface performance, thereby improving the comprehensive performance of the cement paste.
In another technical scheme, the length of the short fiber is 0.1-10 mm.
< example 1>
Step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 10 to prepare a mixed system;
step two, adding epichlorohydrin accounting for 5% of the mass of the sodium alginate into the mixed system, reacting for 3.5 hours at 60 ℃, adding absolute ethyl alcohol, filtering, and drying to obtain crosslinked sodium alginate;
dissolving the crosslinked sodium alginate in water, standing and defoaming to prepare a crosslinked sodium alginate solution with the mass percentage of 3%;
extruding the cross-linked sodium alginate solution into a calcium chloride solution with the mass percent of 4% through a spinneret orifice, wherein the temperature of a coagulating bath is 40 ℃, preparing cross-linked calcium alginate fibers with the average diameter of 200 mu m after traction, water washing and drying, and cutting the cross-linked calcium alginate fibers to the average length of 0.5 mm;
step five, uniformly mixing cement and water to prepare cement slurry, adding 10% of high-strength hollow glass microspheres, 13% of micro-silicon, 1.8% of cross-linked calcium alginate fibers, 0.1% of retarder and 0.1% of dispersant, which account for the mass of the cement, into the cement slurry, and uniformly mixing to prepare the well cementation cement slurry.
< example 2>
Step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 10 to prepare a mixed system;
step two, adding epichlorohydrin accounting for 5% of the mass of the sodium alginate into the mixed system, reacting for 3.5 hours at 60 ℃, adding absolute ethyl alcohol, filtering, and drying to obtain crosslinked sodium alginate;
dissolving the crosslinked sodium alginate in water, standing and defoaming to prepare a crosslinked sodium alginate solution with the mass percent of 4%;
extruding the cross-linked sodium alginate solution into a calcium chloride solution with the mass percent of 3% through a spinneret orifice, wherein the temperature of a coagulating bath is 40 ℃, preparing cross-linked calcium alginate fibers with the average diameter of 200 mu m after traction, water washing and drying, and cutting the cross-linked calcium alginate fibers to the average length of 0.5 mm;
step five, uniformly mixing cement and water to prepare cement paste, taking one fourth of the cement paste, dispersing the crosslinked calcium alginate fibers, the high-strength hollow glass microspheres, the micro-silicon, the retarder and the dispersing agent into the cement paste while stirring, and pre-impregnating by using an ultrasonic impregnation method;
and sixthly, putting the pre-impregnated mixture into the residual cement slurry for fully mixing to prepare the well cementation cement slurry, wherein the mass percentage of each component in the cement is as follows: 20 percent of high-strength hollow glass micro-beads, 15 percent of micro-silicon, 2 percent of cross-linked calcium alginate fiber, 0.1 percent of retarder and 0.1 percent of dispersant.
< example 3>
Step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 10 to prepare a mixed system;
step two, adding epichlorohydrin accounting for 6% of the mass of the sodium alginate into the mixed system, reacting for 3.5 hours at 60 ℃, adding absolute ethyl alcohol, filtering, and drying to obtain crosslinked sodium alginate;
step three, mixing and dissolving crosslinked sodium alginate and sodium carboxymethylcellulose in water according to a molar ratio of 20:3, filtering, standing and defoaming to prepare a mixed spinning solution with the mass percentage of 5%;
step four, taking a calcium chloride solution with the mass percentage of 4% as a coagulating bath, extruding the mixed spinning solution into the coagulating bath through a spinneret orifice, wherein the temperature of the coagulating bath is 40 ℃, then drawing, washing and drying to obtain a cross-linked calcium alginate fiber with the average diameter of 200 mu m, and cutting the cross-linked calcium alginate fiber to the average length of 1 mm;
step five, uniformly mixing cement and water to prepare cement paste, taking one fourth of the cement paste, dispersing the crosslinked calcium alginate fibers, the high-strength hollow glass microspheres, the microsilica, the retarder and the dispersing agent into the cement paste while stirring, and pre-impregnating by using an ultrasonic impregnation method;
and sixthly, putting the pre-impregnated mixture into the residual cement slurry for fully mixing to prepare the well cementation cement slurry, wherein the mass percentage of each component in the cement is as follows: 2 percent of cross-linked calcium alginate fiber, 30 percent of high-strength hollow glass microsphere, 18 percent of micro-silicon, 0.1 percent of retarder and 0.1 percent of dispersant.
< comparative example 1>
The method comprises the following steps of replacing the cross-linked calcium alginate fibers with calcium alginate fibers:
step one, dissolving sodium alginate in water, standing and defoaming to prepare a sodium alginate solution with the mass percentage of 3%;
extruding the sodium alginate solution into a calcium chloride solution with the mass percent of 4% through a spinneret orifice, wherein the temperature of a coagulating bath is 40 ℃, preparing calcium alginate fibers with the average diameter of 200 mu m after traction, water washing and drying, and cutting the calcium alginate fibers to the average length of 0.5 mm;
step three, mixing cement and water uniformly to prepare cement paste, adding 10% of high-strength hollow glass microspheres, 13% of microsilica, 1.8% of cross-linked calcium alginate fibers, 0.1% of retarder and 0.1% of dispersant, which account for the mass of the cement, into the cement paste, and mixing uniformly to prepare the well cementation cement paste.
< comparative example 2>
The cross-linked calcium alginate fiber is replaced by calcium alginate fiber, which is a commercially available G33S common type fluid loss agent, and the specific content is as follows:
the cement and water are mixed evenly to prepare cement paste, 20 percent of high-strength hollow glass micro-beads, 13 percent of micro-silicon, 2 percent of commercially available G33S common type fluid loss additive, 0.1 percent of retarder and 0.1 percent of dispersant which account for the mass of the cement are added into the cement paste and mixed evenly to prepare the well cementation cement paste.
< comparative example 3>
Step one, dissolving sodium alginate in water, filtering, standing and defoaming to prepare a mixed spinning solution with the mass percent of 5%;
step two, taking a calcium chloride solution with the mass percent of 4% as a coagulating bath, extruding the mixed spinning solution into the coagulating bath through a spinneret orifice, and then drawing, washing and drying to obtain calcium alginate fibers;
step three, mixing methanol and water according to the volume ratio of 1:3, adding epoxy chloropropane into the mixed solution, adjusting the pH value to 10 to obtain the product with the concentration of 0.5 multiplied by 10-2mol/L of a crosslinking agent;
soaking the fibers in the cross-linking agent, wherein the volume ratio of the fibers to the cross-linking agent is 1:50, reacting for 3 hours under the condition of constant temperature oscillation at 45 ℃ to obtain cross-linked calcium alginate fibers with the average diameter of 200 mu m, and cutting the cross-linked calcium alginate fibers to the average length of 0.5 mm;
step five, uniformly mixing cement and water to prepare cement slurry, adding 10% of high-strength hollow glass microspheres, 13% of micro-silicon, 1.8% of cross-linked calcium alginate fibers, 0.1% of retarder and 0.1% of dispersant, which account for the mass of the cement, into the cement slurry, and uniformly mixing to prepare the well cementation cement slurry.
< test on Cement mortar Property >
And (3) taking each group of well cementation cement slurry prepared in the examples 1-3 and the comparative examples 1-3, pouring each group of well cementation cement slurry into a pressurization thickening instrument slurry cup according to API (application program interface) specifications, and then placing the slurry cup into a thickening instrument kettle body for thickening experiments. Test conditions for thickening time: 50MPa at 50 ℃. The test results are shown in table 1.
In examples 1-3, high-strength hollow glass microspheres and microsilica are added, so that the density of the cement paste is reduced, and meanwhile, the addition of the crosslinked calcium alginate fibers is matched with other components, so that the density and thickening time of the cement paste are adjustable. In addition, the experiment carries out crosslinking treatment on calcium alginate, so that the strength and the salt resistance of the fiber are improved, and the crosslinked calcium alginate fiber has good hygroscopicity and good stability in saline water. The cross-linked calcium alginate fiber can be adsorbed on the surface of cement particles to form an adsorption hydration layer, so that the cement particles are bridged to form a net structure, more free water is bound, gaps among the cement particles are blocked, the permeability of a cement filter cake is reduced, and the permeability is obviously reduced. Test data show that the technical scheme of the invention has the advantages that the API water loss reaches below 50ml in the environment of fresh water or compound brine, has good water loss control capability and strong salt resistance, and can meet the requirement of target layer well cementation on the water loss rate.
TABLE 1
< Cement Strength test >
Performing a set cement strength determination test on the well cementation cement slurry prepared in the examples 1-3 and the comparative examples 1-3 by using GB/T19139-2012, wherein the set cement curing conditions are as follows: 60 ℃ X21 MPa X7 d. The test data are shown in table 2:
TABLE 2
The test results show that the cement paste in examples 1-3 has good compressive strength, because the micro-silicon and high-strength hollow glass bead particles are fine and can be fully and effectively filled among the cement particles, the gaps among the cement, the micro-silicon and high-strength hollow glass bead particles are reduced, and the addition of the cross-linked calcium alginate fibers ensures that the cement paste can be well and compactly cemented in the coagulation process, so that the compressive strength is improved. Compared with other low-density cements, the cement paste in examples 1-3 has the obvious characteristics of tight embedding among particles, tiny pores and high strength, which are different from other low-density cements.
In addition, the brittleness coefficient of the example 3 is the minimum, and better toughness is reflected, because the calcium alginate and the carboxymethyl cellulose are blended and crosslinked in the example 3, the prepared crosslinked calcium alginate fiber has good flexibility and hygroscopicity, and meanwhile, the crosslinked calcium alginate fiber, the high-strength hollow glass microspheres, the microsilica, the retarder and the dispersing agent are ultrasonically impregnated in a small amount of cement in advance through an ultrasonic impregnation technology, so that the binding property of each component in the cement is improved, and the comprehensive performance of the mixed cement slurry is improved.
Therefore, the technical scheme of the invention can reduce the density of the well cementation cement slurry, can adjust the density and the thickening time, has high strength, low filtration vector, no toxicity, no pollution, environmental protection and degradability, and can meet the well cementation construction process requirement of a low-pressure stratum easy to leak.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the examples shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (8)
1. The well cementation cement additive is characterized by comprising the following components in percentage by mass of cement: 2-35% of high-strength hollow glass beads, 1-20% of micro-silicon, 0.02-10% of cross-linked calcium alginate fibers, 0.01-3% of retarder and 0.01-3% of dispersant;
the preparation method of the cross-linked calcium alginate fiber comprises the following steps:
step one, mixing sodium alginate and water in a mass ratio of 1:10, and adjusting the pH value to 8-10 to prepare a mixed system;
step two, adding epoxy chloropropane accounting for 3-7% of the mass of the sodium alginate into the mixed system, reacting for 1.5-3.5 h at 40-60 ℃, adding absolute ethyl alcohol, performing suction filtration, and drying to obtain the cross-linked sodium alginate;
dissolving the crosslinked sodium alginate in water, standing and defoaming to prepare a crosslinked sodium alginate solution with the mass percent of 3-5%;
extruding the cross-linked sodium alginate solution into a coagulating bath of 1-5% calcium chloride solution by mass percent through a spinneret orifice, wherein the temperature of the coagulating bath is 40 ℃, and obtaining the cross-linked calcium alginate fiber after traction, water washing and drying.
2. The cement additive of claim 1, wherein the pH is adjusted to 10 in step one.
3. The cement additive for well cementation according to claim 1, wherein epichlorohydrin in step two accounts for 5% by mass of sodium alginate.
4. The cement additive for well cementation according to claim 1, wherein the diameter of the cross-linked calcium alginate fiber is 100 to 600 μm.
5. The cement additive for well cementation according to claim 1, wherein the high strength hollow glass beads have an average diameter of 0.2 to 0.3 μm.
6. The cement additive for well cementation according to claim 1, wherein the microsilica has an average diameter of 0.05 to 0.3 μm.
7. The method for using the cement additive for well cementation according to claim 1, characterized by comprising the following steps:
step one, mixing cement and water uniformly to prepare cement paste;
cutting the cross-linked calcium alginate fibers into short fibers;
taking quarter of cement paste, stirring and dispersing the short fibers, the high-strength hollow glass microspheres, the micro-silicon, the retarder and the dispersing agent into the cement paste, and pre-impregnating by using an ultrasonic impregnation method;
and step four, putting the pre-impregnated mixture into the residual cement slurry for fully mixing to prepare the well cementation cement slurry.
8. The method for using the cement additive for well cementation according to claim 7, wherein the length of the short fiber is 0.1 to 10 mm.
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| CN102382632A (en) * | 2010-09-03 | 2012-03-21 | 中国石油化工股份有限公司 | Pretreating agent preventing leaking stoppage from being diluted by formation water and preparation method and application thereof |
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| CN111849440A (en) * | 2020-06-29 | 2020-10-30 | 尧柏特种水泥技术研发有限公司 | Low-thixotropic low-density oil well cement slurry for oil and gas well cementing treatment |
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| US20070267598A1 (en) * | 2006-05-22 | 2007-11-22 | Artmolds, Inc. | Non-silica containing impression and casting materials |
| US20180002596A1 (en) * | 2015-01-16 | 2018-01-04 | Schlumberger Technology Corporation | Subterranean fluids containing suspended polymer bodies |
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| CN102382632A (en) * | 2010-09-03 | 2012-03-21 | 中国石油化工股份有限公司 | Pretreating agent preventing leaking stoppage from being diluted by formation water and preparation method and application thereof |
| CN104559973A (en) * | 2013-10-28 | 2015-04-29 | 德惠同利（北京）石油技术服务有限公司 | Elastic plugging agent |
| CN104263332A (en) * | 2014-10-08 | 2015-01-07 | 中钢集团马鞍山矿山研究院有限公司 | High-temperature-resistant high-strength low-density well-cementing cement slurry |
| CN106521707A (en) * | 2016-11-25 | 2017-03-22 | 陕西品达石化有限公司 | Preparation method of epichlorohydrin crosslinked sodium alginate fiber |
| CN111849440A (en) * | 2020-06-29 | 2020-10-30 | 尧柏特种水泥技术研发有限公司 | Low-thixotropic low-density oil well cement slurry for oil and gas well cementing treatment |
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