CN115504700B - Preparation method of oil well cement expanding agent - Google Patents
Preparation method of oil well cement expanding agent Download PDFInfo
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- CN115504700B CN115504700B CN202211203119.XA CN202211203119A CN115504700B CN 115504700 B CN115504700 B CN 115504700B CN 202211203119 A CN202211203119 A CN 202211203119A CN 115504700 B CN115504700 B CN 115504700B
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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
- 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
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- 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
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
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Abstract
The invention relates to a preparation method of an oil well cement expanding agent, which sequentially comprises the following steps: s1, grinding dolomite, calcium stearate and magnesium stearate by a ball mill, stirring, and then mixing with diatomite; s2, sequentially drying and tabletting the mixed materials to obtain a test piece; s3, presintering the test piece, cooling and crushing to obtain powder; s4, calcining the powder at a high temperature, preserving heat for a period of time, and quenching to obtain an expanding agent block; s5, grinding the expansion agent block body through a ball mill to obtain the cement expansion agent. The method is reliable in principle and simple and convenient to operate, and the expansion agent is prepared by blending dolomite into diatomite, so that the volume shrinkage in the cement hydration process is reduced, the interlayer sealing capacity of the well cementation cement sheath is improved, the occurrence of channeling is prevented, and the well cementation cement sheath is guaranteed to have good integrity.
Description
Technical Field
The invention relates to a preparation method of an oil well cement expanding agent, belonging to the field of oil and gas well cementing cement slurry additives.
Background
Cementing is an indispensable part of drilling operation, and the main process comprises casing running and cementing, so as to seal the annular space between the casing and the well wall, form a cement sheath with high compressive strength and high cementing capacity, and prevent underground fluid from flowing along the cement sheath in the well. The high-pressure gas of stratum invades the cement paste column in the cementing process to cause gas channeling, so that pollution and loss of oil and gas resources can be caused, the method is one of the major problems which are not completely solved in the current cementing operation at home and abroad, and even the oil and gas well cannot be put into production when the gas channeling is serious. The cement commonly used in the well cementation operation is silicate cement, the cement paste has large water-cement ratio, high service temperature and pressure, and large shrinkage rate in use, and is a main cause of annulus channeling, easy shrinkage cracking of cement sheath and unqualified well cementation quality.
The use of an oil well cement expanding agent is an important means to prevent gas channeling and to avoid shrinkage cracking of the oil well cement sheath, with the purpose of compensating for the volumetric shrinkage of the cement and causing it to expand slightly. Existing expanding agents can be divided into two major classes, namely gas-generating expanding agents (hydrogen, nitrogen and the like) and crystal expanding agents (expanding agents ettringite, calcium oxide, magnesium oxide and the like). The gas-generating expanding agent mainly takes gas generated by the reaction of alkali active metal powder and alkali solution in cement slurry as an expansion source, is suitable for low-pressure environment and shallow wells, has the gas-generating time controlled by temperature and has a narrow application range. The crystal expanding agent mainly compensates volume shrinkage generated during cement hardening and improves the cement stone structure to a certain extent through the generation of the ettringite, the calcium hydroxide and the magnesium hydroxide. Wherein the solubility of the ettringite and the calcium hydroxide is larger and the stability is poorer under the action of the pressure in the well (the ettringite can be decomposed at the temperature of more than 70 ℃).
The MgO expanding agent is a novel crystal expanding agent, and has the advantages of less hydration water, adjustable expansion process, stable hydration products and the like compared with the traditional expanding agent taking ettringite as an expansion source, but the root cause of the expansion of the MgO expanding agent in cement concrete is the hydration of MgO, and the MgO can be hydrated in advance due to the overhigh temperature in the use process of well cementation cement paste, so that the expansion agent has large early expansion rate and small later expansion rate, and the expansion stability is advanced. The diatomite particles have more pores and larger specific surface area, and can absorb some free water in the slurry, so that the free water content is reduced, and the slurry is thickened. By fully utilizing the characteristics, mgO is doped into the diatomite pores to be combined with cement paste, so that the crack resistance of the well cementation cement stone is improved, and the purposes of improving the well cementation quality and ensuring the integrity of the well cementation shaft cement stone are realized.
Disclosure of Invention
The invention aims to provide a preparation method of an oil well cement expanding agent, which has the advantages of reliable principle and simple and convenient operation, and the expanding agent is prepared by blending dolomite into diatomite, so that the volume shrinkage in the cement hydration process is reduced, the interlayer sealing capacity of a well cementation cement ring is improved, the occurrence of cross flow is prevented, and the well cementation cement ring is ensured to have better integrity.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
The preparation method of the oil well cement expanding agent sequentially comprises the following steps:
s1, grinding dolomite, calcium stearate and magnesium stearate by a ball mill, stirring, and then mixing with diatomite;
s2, sequentially drying and tabletting the mixed materials to obtain a test piece;
s3, presintering the test piece, cooling and crushing to obtain powder;
s4, calcining the powder at a high temperature, preserving heat for a period of time, and quenching to obtain an expanding agent block;
s5, grinding the expansion agent block body through a ball mill to obtain the cement expansion agent.
In the step S1, the dolomite, the calcium stearate and the magnesium stearate are ground by a ball mill to have the average particle size of 1500-3200 meshes, the ground magnesium stearate and the ground calcium stearate are added into the ground dolomite and stirred for 30-90 min, and then the mixture is mixed with diatomite, wherein the mass ratio of the diatomite to the dolomite to the calcium stearate to the magnesium stearate is 180-240: 80-150: 3-8: 3 to 9.
The mean particle size of the dolomite, calcium stearate and magnesium stearate after grinding is preferably 2500 mesh (i.e. 5 μm).
The mass ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is preferably 190-220: 90-120: 4 to 6:4 to 7.
In the step S2, the drying conditions are as follows: drying at 90deg.C with box blower for 12 hr; the tabletting conditions are as follows: the pressure is 50-65 KN, the pressure increasing rate is 0.2KN/s, the pressure is relieved after 185-200 s of pressure maintaining, and the pressure is less than or equal to 4.5KN during pressure relief.
In the step S3, the step of pre-sintering is as follows: the temperature is between room temperature and 650 ℃ and the temperature rising time is between 35 and 55 minutes; the temperature is 650 ℃ and the heat preservation time is 5-20 min; the temperature is 650-800 ℃ and the heating time is 30-45 min; the temperature is raised for 30min at 800-900 ℃ and the heat preservation time is 50-120 min; the cooling mode is natural cooling or wind cooling; the crushing mode is jet milling or ball milling crushing, and the particle size of the crushed powder is 1500-3200 meshes.
In the step S4, the conditions of the high-temperature calcination are as follows: calcining in a muffle furnace at 900-1100 ℃ for 20-35 s; the heat preservation time is 30-120 min; the quenching adopts a liquid nitrogen quenching mode.
In the step S5, the particle size of the expansion agent block after being ground by a ball mill is 1500-3200 mesh.
The cement expanding agent is added into oil well cement to obtain well cementation cement with good gas channeling prevention and crack resistance.
The mass percentage of the cement expanding agent in the oil well cement is 4-5%.
The oil well cement is G-grade oil well cement or Portland cement. Both are the most commonly used cements in oil and gas cementing construction processes.
The preparation of the well cementation cement also needs to add conventional additives and external additives, such as dispersing agents, fluid loss agents, defoaming agents and the like, and is determined according to specific requirements.
The well cementation cement added with the expanding agent is particularly suitable for well cementation operation with strict requirements on gas channeling prevention and crack resistance, not only can improve the crack resistance of cement stones, but also can improve the interlayer sealing capacity of cement rings, prevent channeling and ensure that cement rings have better integrity.
Compared with the prior art, the invention has the following beneficial effects:
(1) The expanding agent combines diatomite with MgO and CaO by adopting a two-step sintering process, the diatomite is porous and poor in fluidity, and MgO and CaO are fused into the pores of the diatomite by the method, so that the fluidity of the diatomite is improved, the consistency of cement paste is increased, and all performances of the diatomite and the CaO are improved.
(2) The expanding agent adopts dolomite as a raw material, mgO and CaO in diatomite micropores are derived from all raw materials, and the purity and chemical stability of the product are ensured; and the particle size of the crushed material is 1500-3200 meshes, and the specific surface area is large, so that the raw materials can fully react in the high-temperature calcination process.
(3) The swelling agent has slow hydration reaction process, can enable cement to carry out hydration reaction again in the later stage, controls the swelling time of MgO, enables the MgO to react in the required time, and achieves the purposes of preventing channeling and cracking in the later stage.
(4) When the expanding agent and cement slurry are hydrated, firstly, the cement clinker is hydrated to generate Ca (OH) 2 、Mg(OH) 2 Then the Ca (OH) is generated 2 、Mg(OH) 2 The calcium silicate hydrate, the magnesium silicate hydrate, the calcium aluminate hydrate or the magnesium aluminate hydrate are alternately carried out, so that the microstructure of the cement can be improved, and the strength of the cement can be improved.
(5) The preparation method provided by the invention has the advantages of reliable technology, high yield and lower quality requirement on raw materials; the prepared product has high uniformity, good chemical stability and strong hydration capacity, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a volume shrinkage chart of the set cement of example 1.
FIG. 2 is a volume shrinkage chart of the set cement of example 2.
FIG. 3 is a volume shrinkage chart of the set cement of example 3.
Fig. 4 is a volume shrinkage chart of set cement without an expanding agent.
Detailed Description
The invention is further described below with reference to the drawings and examples to facilitate an understanding of the invention by those skilled in the art. It should be understood that the invention is not limited to the precise embodiments, and that various changes may be effected therein by one of ordinary skill in the art without departing from the spirit or scope of the invention as defined and determined by the appended claims.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
The composition of the expanding agent in this example is as follows:
the weight ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 200:120:6:5.
grinding dolomite, calcium stearate and magnesium stearate for 6 hours respectively by adopting a ball mill, adding the ground calcium stearate and magnesium stearate into the ground dolomite, stirring for 40min, and then mixing with diatomite to obtain the raw material. Drying the raw materials, tabletting the dried raw materials (the pressure is 50KN, the boosting rate is 0.2KN/s, the pressure is reduced after the pressure is maintained for 185s, and the pressure is less than or equal to 4.5KN during the pressure reduction). The test piece obtained by pressing is placed in a crucible and presintered by a resistance furnace (the temperature rising and heat preserving process is that the room temperature is between 650 ℃ and the temperature rising time is 35min, the temperature rising time is 650 ℃, the heat preserving time is 10min, the temperature rising time is 650-800 ℃, the temperature rising time is 30min, the temperature rising time is 800-900 ℃, the temperature rising time is 30min, the heat preserving time is 55 min), the presintered product is forcedly cooled by cold air and then crushed, and the particle size is controlled to be 1500-3200 meshes. Calcining the crushed presintered product in a muffle furnace, controlling the flame temperature to 900 ℃, the calcining time to 25s, immediately quenching the product with liquid nitrogen after heat preservation for 100min, and grinding the expanding agent block to 1500-3200 meshes by a ball mill to obtain the cement expanding agent material.
Example 2
The composition of the expanding agent in this example is as follows:
the weight ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 190:90:5:4.
grinding dolomite, calcium stearate and magnesium stearate for 6 hours respectively by adopting a ball mill, adding the ground calcium stearate and magnesium stearate into the ground dolomite, stirring for 60 minutes, and then mixing with diatomite to obtain the raw material. Drying the raw materials, tabletting the dried raw materials (the pressure is 60KN, the pressure increasing rate is 0.2KN/s, the pressure is reduced after the pressure is maintained for 190s, and the pressure is less than or equal to 4.5KN during the pressure reduction). The test piece obtained by pressing is placed in a crucible and presintered by a resistance furnace (the heating and heat preservation process is that the room temperature is between 650 ℃ and the temperature is between 45 minutes, the heating time is 650 ℃, the heat preservation time is 15 minutes, the heating time is between 650 and 800 ℃, the heating time is 40 minutes, the heating time is between 800 and 900 ℃, the heating time is 30 minutes, the heat preservation time is 90 minutes), the presintered product is forcedly cooled by cold air and then crushed, and the particle size is controlled to be 1500 to 3200 meshes. Calcining the crushed presintered product in a muffle furnace, controlling the flame temperature to be 1000 ℃, the calcining time to be 28s, immediately quenching the product with liquid nitrogen after heat preservation for 80min, and grinding the expanding agent block to 1500-3200 meshes by a ball mill to obtain the cement expanding agent material.
Example 3
The composition of the expanding agent in this example is as follows:
the weight ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 210:110:4:7.
grinding dolomite, calcium stearate and magnesium stearate for 6 hours respectively by adopting a ball mill, adding the ground calcium stearate and magnesium stearate into the ground dolomite, stirring for 80 minutes, and then mixing with diatomite to obtain the raw material. Drying the raw materials, tabletting the dried raw materials (the pressure is 65KN, the boosting rate is 0.2KN/s, the pressure is reduced after the pressure is maintained for 200 seconds, and the pressure is less than or equal to 4.5KN during the pressure reduction). The test piece obtained by pressing is placed in a crucible and presintered by a resistance furnace (the temperature rising and heat preserving process is that the room temperature is between 650 ℃ and the temperature rising time is 55min, the temperature rising time is 650 ℃ and the heat preserving time is 20min, the temperature rising time is 650-800 ℃ and 45min, the temperature rising time is 800-900 ℃ and the temperature rising time is 30min, the heat preserving time is 120 min), the presintered product is forcedly cooled by cold air and then crushed, and the particle size is controlled to be 1500-3200 meshes. Calcining the crushed presintered product in a muffle furnace, controlling the flame temperature to be 1100 ℃, the calcining time to be 35s, immediately quenching the product with liquid nitrogen after heat preservation for 60min, and grinding the expanding agent block to 1500-3200 meshes through a ball mill to obtain the cement expanding agent material.
The prepared cement paste is directly poured into a paste cup with the volume of 240ml and is put into a high-temperature high-pressure volume change rate testing device to test the volume shrinkage performance, and experimental parameters and experimental results are shown in table 1.
TABLE 1 set of set-cement parameters and results for volume shrinkage test
After the volume of the cement stone is shrunk, the cementing quality of a first interface and a second interface of the well cementation is reduced, and micro annular gaps and micro cracks are formed at the interfaces, so that a channel is provided for the channeling of gas, and the channeling of gas is caused. The greater the volume shrinkage, the greater the likelihood of microcirculatory voids and microcracks and gas channeling. The experiments showed that the volume shrinkage of the set cement without the expanding agent was 0.60178%, and the volume shrinkage of the set cement of examples 1, 2 and 3 was 0.01269%, 0.06954% and 0.02821%, respectively, as shown in table 1.
The formula of the cement paste is as follows: 100 parts of G oil well cement, 0.5 part of dispersant USZ (Henan Wei Hui chemical Co., ltd.), 2 parts of fluid loss agent G33S (Henan Wei Hui chemical Co., ltd.), 0.01 part of oil well cement defoamer XP-I (Henan Wei Hui chemical Co., ltd.), 2 parts of swelling agent and 44 parts of water. Cement slurries and set cements were prepared according to GB/T19139-2012 method for testing oil well cement.
The volume shrinkage maps of examples 1 to 3 are shown in fig. 1 to 3, and fig. 4 is a volume shrinkage map without an expanding agent.
As can be seen from an analysis of the experimental results of fig. 1 to 4: the cement stone for well cementation without adding the expanding agent is easy to shrink and crack when being cured for 24 hours under the condition of 60 ℃ (clean water) and solidified, the volume rate of the cement stone begins to become larger at 7 hours. After the cement stone is cured for 24 hours under the condition of 60 ℃ (clean water), the volume shrinkage of the cement stone is smaller and basically kept stable, which indicates that the volume shrinkage of the cement stone is compensated by adding the expansion agent, and the crack resistance of the cement stone is ensured.
Claims (6)
1. The preparation method of the oil well cement expanding agent sequentially comprises the following steps:
s1, grinding dolomite, calcium stearate and magnesium stearate by a ball mill, wherein the average particle size is 1500-3200 meshes, adding the ground magnesium stearate and calcium stearate into the ground dolomite, stirring for 30-90 min, mixing with diatomite after stirring, and the mass ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 180-240: 80-150: 3-8: 3-9;
s2, sequentially drying and tabletting the mixed materials to obtain a test piece;
s3, pre-sintering the test piece, cooling and crushing to obtain powder, wherein the pre-sintering step is as follows: the temperature is between room temperature and 650 ℃ and the temperature rising time is between 35 and 55 minutes; the temperature is 650 ℃ and the heat preservation time is 5-20 min; the temperature is 650-800 ℃ and the heating time is 30-45 min; the temperature is 800-900 ℃, the heating time is 30min, and the heat preservation time is 50-120 min;
s4, calcining the powder at a high temperature, and quenching after heat preservation for a period of time to obtain an expanding agent block, wherein the conditions of the high temperature calcination are as follows: calcining in a muffle furnace at 900-1100 ℃ for 20-35 s; the heat preservation time is 30-120 min;
s5, grinding the expansion agent block body through a ball mill to obtain the cement expansion agent.
2. The method for preparing an oil well cement expanding agent according to claim 1, wherein in the step S1, the average particle size of the ground dolomite, calcium stearate and magnesium stearate is 2500 mesh.
3. The method for preparing the oil well cement expanding agent according to claim 1, wherein in the step S1, the mass ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 190-220: 90-120: 4-6: 4-7.
4. The method for preparing an oil well cement expanding agent according to claim 1, wherein in the step S2, the drying condition is as follows: drying at 90deg.C with box blower for 12 hr; the tabletting conditions are as follows: the pressure is 50-65 kN, the boosting rate is 0.2kN/s, the pressure is relieved after 185-200 s of pressure maintaining, and the pressure is less than or equal to 4.5kN during pressure relief.
5. The method for preparing an oil well cement expanding agent according to claim 1, wherein in the step S5, the particle size of the expanding agent block is 1500-3200 mesh after being ground by a ball mill.
6. The method for preparing the oil well cement expanding agent according to claim 1, 2, 3, 4 or 5, wherein the prepared cement expanding agent is added into oil well cement to obtain well cement with good gas channeling prevention and crack resistance, and the mass percentage of the cement expanding agent in the oil well cement is 4-5%.
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