CN115504700A - Preparation method of oil well cement expanding agent - Google Patents
Preparation method of oil well cement expanding agent Download PDFInfo
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- CN115504700A CN115504700A CN202211203119.XA CN202211203119A CN115504700A CN 115504700 A CN115504700 A CN 115504700A CN 202211203119 A CN202211203119 A CN 202211203119A CN 115504700 A CN115504700 A CN 115504700A
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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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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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
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 mixing with diatomite; s2, drying and tabletting the mixed materials in sequence to obtain test pieces; s3, pre-sintering the test piece, cooling and crushing to obtain powder; s4, calcining the powder at a high temperature, and quenching after keeping the temperature for a period of time to obtain an expanding agent block; and S5, grinding the expanding agent block by using a ball mill to obtain the cement expanding agent. The invention has reliable principle and simple and convenient operation, reduces the volume shrinkage in the cement hydration process and improves the sealing capability between the layers of the well cementation cement sheath by preparing the expanding agent by blending the dolomite into the diatomite, thereby preventing the occurrence of channeling and ensuring the good integrity of the well cementation cement sheath.
Description
Technical Field
The invention relates to a preparation method of an oil well cement expanding agent, belonging to the field of additives of oil and gas well cementing cement slurry.
Background
The well cementation is an indispensable part of the well drilling operation, the main process comprises casing setting and cement injection, the aim is to seal the annular space between the casing and the well wall to form a cement sheath with high compressive strength and high cementing capacity, and the channeling of underground fluid along the cement sheath in the well is prevented. In the cementing process, stratum high-pressure gas invades a cement column to cause gas channeling, so that oil and gas resources are polluted and lost, the cementing device is one of major problems which are not completely solved in the cementing operation at home and abroad at present, and an oil and gas well can not even be put into production when the gas channeling is serious. The cement commonly used in well cementation operation is silicate cement, the cement paste has large water-cement ratio and high service temperature and pressure, and has large shrinkage rate in use, so that the cement paste is the main reason for causing annular flow channeling, easy shrinkage cracking of a cement sheath and unqualified well cementation quality.
The use of an oil well cement swelling agent is an important means for preventing gas channeling and preventing shrinkage cracking of an oil well cement sheath, and the purpose of the agent is to compensate for the volume shrinkage of cement and to slightly swell the cement. The existing expanding agents can be divided into two main types of gas-generating expanding agents (hydrogen, nitrogen and the like) and crystal expanding agents (expanding agents such as ettringite, calcium oxide, magnesium oxide and the like). The gas generating type expanding agent mainly takes gas generated by reaction of alkali active metal powder and an alkali solution in cement paste as an expansion source, is suitable for low-pressure environments and shallow wells, is controlled by temperature in gas generating time, and is narrow in application range. The crystal expanding agent compensates volume shrinkage occurring when cement is hardened and improves a cement stone structure to a certain extent mainly by generating ettringite, calcium hydroxide and magnesium hydroxide. The ettringite and calcium hydroxide have high solubility and poor stability under the action of pressure in the well (the ettringite is decomposed at a temperature of more than 70 ℃).
The MgO expanding agent is a novel crystal expanding agent, and compared with the traditional expanding agent taking ettringite as an expansion source, the MgO expanding agent has the advantages of small water requirement for hydration, adjustable expansion process, stable hydration products and the like, but the basic reason for the expansion of the MgO expanding agent in cement concrete is the hydration of MgO, and in the using process of well cementation cement slurry, because the temperature is too high, the MgO can be hydrated in advance, so that the expansion rate of the expanding agent in the early stage is high, the expansion rate of the expanding agent in the later stage is low, and the expansion stability period is advanced. The diatomite particles have more pores and larger specific surface area, and can absorb some free water in the slurry, thereby reducing the free water content and thickening the slurry. By fully utilizing the characteristics, mgO is doped into the diatomite pores to be combined with cement slurry, which is beneficial to improving the crack resistance of the well cementation set cement, thereby realizing the purposes of improving the well cementation quality and ensuring the integrity of the well cementation shaft set cement.
Disclosure of Invention
The invention aims to provide a preparation method of an oil well cement expanding agent, which has reliable principle and simple and convenient operation, reduces volume shrinkage in the cement hydration process and improves the interlayer sealing capability of a well cementation cement sheath by blending dolomite into diatomite to prepare the expanding agent, thereby preventing the occurrence of channeling and ensuring that the well cementation cement sheath has better integrity.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
A preparation method of an oil well cement expanding agent sequentially comprises the following steps:
s1, grinding dolomite, calcium stearate and magnesium stearate by a ball mill, stirring, and mixing with diatomite;
s2, drying and tabletting the mixed materials in sequence to obtain test pieces;
s3, pre-sintering the test piece, cooling and crushing to obtain powder;
s4, calcining the powder at a high temperature, and quenching after keeping the temperature for a period of time to obtain an expanding agent block;
and S5, grinding the expanding agent block by using a ball mill to obtain the cement expanding agent.
In the step S1, the dolomite, the calcium stearate and the magnesium stearate are ground by a ball mill, the average grain diameter is 1500-3200 meshes, the ground magnesium stearate and the calcium stearate are added into the ground dolomite to be stirred for 30-90 min, and are mixed with the diatomite after stirring, wherein the mass ratio of the diatomite to the dolomite to the calcium stearate to the magnesium stearate is 180-240: 80 to 150:3 to 8:3 to 9.
The dolomite, calcium stearate and magnesium stearate preferably have an average particle size of 2500 mesh (i.e., 5 μm) after grinding.
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 90 deg.C for 12 hr with box blower; the tabletting conditions were: the pressure is 50-65 KN, the boosting rate is 0.2KN/s, the pressure is relieved after the pressure is maintained for 185-200 s, and the pressure is less than or equal to 4.5KN when the pressure is relieved.
In the step S3, the pre-sintering step is as follows: the room temperature is 650 ℃, and the temperature rise time is 35-55 min; keeping the temperature at 650 ℃ for 5-20 min; the temperature is raised for 30-45 min at 650-800 ℃; the temperature is increased 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 air flow crushing or ball milling crushing, and the particle size of the crushed powder is 1500-3200 meshes.
In the step S4, the high-temperature calcination conditions are as follows: calcining in a muffle furnace at the temperature of 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 bulk expanding agent after being ground by the ball mill is 1500 to 3200 meshes.
The cement expansion agent is added into oil well cement to obtain well cementation cement with good gas channeling prevention and cracking 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 applied cements in oil and gas cementing construction processes.
The well cementation cement is prepared by adding conventional additives and external additives such as a dispersing agent, a fluid loss agent, a defoaming agent and the like according to specific needs.
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, can improve the crack resistance of set cement, can also improve the interlayer sealing capacity of a cement sheath, prevents channeling, and ensures that the cement sheath has better integrity.
Compared with the prior art, the invention has the following beneficial effects:
(1) The expanding agent adopts a two-step sintering process to combine the diatomite with the MgO and the CaO, the diatomite is porous and has poor fluidity, the MgO and the CaO are fused into the pores of the diatomite by the method, so that the fluidity of the diatomite becomes good, the consistency of cement paste is increased, and various performances of the diatomite and the diatomite are improved.
(2) The expanding agent adopts dolomite as a raw material, and MgO and CaO in micropores of the diatomite are derived from all the raw materials, so that the purity and the chemical stability of a product are ensured; the particle size of the crushed material is 1500-3200 meshes, and the specific surface area is large, so that the raw material can fully react in the high-temperature calcination process.
(3) The swelling agent provided by the invention has a slow hydration reaction process, can enable the cement to be subjected to hydration reaction again in a later period, controls the swelling time of MgO, enables the MgO to react in a required time, and achieves the purposes of preventing channeling and resisting cracking in the later period.
(4) When the swelling agent related by the invention is hydrated with cement paste, firstly, the cement clinker is hydrated to generate Ca (OH) 2 、Mg(OH) 2 Then Ca (OH) formed 2 、Mg(OH) 2 The active components such as active silicon dioxide, active alumina and the like in the diatomite are subjected to pozzolan reaction to generate reaction products such as hydrated calcium silicate, hydrated magnesium silicate, hydrated calcium aluminate or hydrated magnesium aluminate, and the like, and the two reactions 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 requirement on the quality of raw materials; the prepared product has high uniformity, good chemical stability and strong hydration capability, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a graph showing the volumetric shrinkage of set cement of example 1.
FIG. 2 is a graph showing the volumetric shrinkage of set cement of example 2.
FIG. 3 is a volume shrinkage plot of set cement of example 3.
FIG. 4 is a graph of the volumetric shrinkage of set cement without the addition of an expansion agent.
Detailed Description
The invention is further illustrated below with reference to the figures and examples in order to facilitate the understanding of the invention by a person skilled in the art. It is to be understood that the invention is not limited in scope to the specific embodiments, but is intended to cover various modifications within the spirit and scope of the invention as defined and defined by the appended claims, as would be apparent to one of ordinary skill in the art.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples 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 to the dolomite to the calcium stearate to the magnesium stearate is 200:120:6:5.
respectively grinding dolomite, calcium stearate and magnesium stearate for 6 hours by adopting a ball mill, adding the ground calcium stearate and magnesium stearate into the ground dolomite, stirring for 40min, and mixing with diatomite to obtain the raw material. Drying the raw materials, and tabletting the dried raw materials (the pressure is 50KN, the boosting rate is 0.2KN/s, the pressure is maintained for 185s, and then the pressure is released, wherein the pressure is less than or equal to 4.5KN when the pressure is released). Placing the test piece obtained by pressing in a crucible and presintering by using a resistance furnace (the temperature rise and heat preservation processes are that the temperature rise is between room temperature and 650 ℃, the temperature rise time is 35min, the temperature preservation time is 10min, the temperature rise time is 650-800 ℃, the temperature rise time is 30min, the temperature rise time is 30min, and the heat preservation time is 55 min), forcibly cooling a presintering product by using cold air, and then crushing the presintering product, wherein the particle size is controlled to be 1500-3200 meshes. And calcining the crushed pre-sintered product in a muffle furnace, controlling the flame temperature at 900 ℃ and the calcining time at 25s, immediately performing liquid nitrogen shock cooling on the product after heat preservation for 100min, and grinding the expanding agent block to 1500-3200 meshes by using 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.
respectively grinding dolomite, calcium stearate and magnesium stearate for 6 hours by adopting a ball mill, adding the ground calcium stearate and magnesium stearate into the ground dolomite, stirring for 60min, and mixing with diatomite to obtain the raw material. Drying the raw materials, and tabletting the dried raw materials (the pressure is 60KN, the boosting rate is 0.2KN/s, the pressure is released after the pressure is maintained for 190s, and the pressure is less than or equal to 4.5KN when the pressure is released). Placing the test piece obtained by pressing in a crucible and presintering by using a resistance furnace (the temperature rise and heat preservation processes are that the temperature rise is 650 ℃ to 650 ℃, the temperature rise time is 45min, the heat preservation time is 15min, the temperature rise time is 650 to 800 ℃, the temperature rise time is 40min to 900 ℃, the temperature rise time is 30min, and the heat preservation time is 90 min), forcibly cooling the presintering product by using cold air, and then crushing the presintering product, wherein the particle size is controlled to be 1500-3200 meshes. And calcining the crushed pre-sintered product in a muffle furnace, controlling the flame temperature to be 1000 ℃, calcining for 28s, immediately performing liquid nitrogen quenching on the product after heat preservation for 80min, and grinding the expanding agent block to 1500-3200 meshes by using 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.
respectively grinding dolomite, calcium stearate and magnesium stearate for 6 hours by adopting a ball mill, adding the ground calcium stearate and magnesium stearate into the ground dolomite, stirring for 80min, and mixing with diatomite to obtain the raw material. Drying the raw materials, and tabletting the dried raw materials (pressure is 65KN, boosting rate is 0.2KN/s, pressure is maintained for 200s, and then pressure is released, wherein the pressure is less than or equal to 4.5KN when pressure is released). Placing the test piece obtained by pressing in a crucible and pre-sintering by using a resistance furnace (the temperature rise and heat preservation processes are that the temperature rise is between room temperature and 650 ℃, the temperature rise time is 55min, the temperature preservation time is between 650 and 800 ℃, the temperature rise time is between 800 and 900 ℃, the temperature rise time is 30min, and the heat preservation time is 120 min), forcibly cooling the pre-sintered product by using cold air, and then crushing the pre-sintered product, wherein the particle size is controlled to be between 1500 and 3200 meshes. And calcining the crushed pre-sintered product in a muffle furnace, controlling the flame temperature at 1100 ℃ and the calcining time at 35s, immediately performing liquid nitrogen quenching on the product after keeping the temperature for 60min, and grinding the expanding agent block to 1500-3200 meshes by using a ball mill to obtain the cement expanding agent material.
The prepared cement slurry is directly poured into a slurry cup with the volume of 240ml and is placed into a high-temperature high-pressure volume change rate testing device to test the volume shrinkage performance, and the experimental parameters and the experimental results are shown in table 1.
TABLE 1 set of Cement volume shrinkage test parameters and results
After the cement stone is subjected to volume shrinkage, the cementing quality of a first interface and a second interface of a well cementation is reduced, and micro annular gaps and micro cracks are formed at the interfaces, so that a channel is provided for gas channeling, and the gas channeling is caused. The greater the volume shrinkage, the greater the probability of micro-annuli and micro-cracks and gas channeling. From experiments, it is found that the volume shrinkage of the set cement without the addition of the expanding agent is 0.60178%, and from table 1, the volume shrinkage of the set cement of examples 1, 2 and 3 is 0.01269%, 0.06954% and 0.02821%, respectively.
The formula of the cement paste is as follows: 100 parts of G oil well cement, 0.5 part of dispersing agent USZ (Henan Wei Hui chemical industry Co., ltd.), 2 parts of fluid loss additive G33S (Henan Wei Hui chemical industry Co., ltd.), 0.01 part of oil well cement defoaming agent XP-I (Henan Wei Hui chemical industry Co., ltd.), 2 parts of expanding agent and 44 parts of water. Preparing cement paste and curing set cement according to GB/T19139-2012 'oil well cement test method'.
The volume shrinkage diagrams of examples 1 to 3 are shown in FIGS. 1 to 3, and FIG. 4 is a volume shrinkage diagram without adding an expanding agent.
As can be seen from an analysis of the experimental results of fig. 1 to 4: when the well cementation set cement without the addition of the expanding agent is cured for 24 hours under the condition of 60 ℃ (clear water) and solidified, the volume ratio of the set cement begins to increase after 7 hours, and the set cement is easy to shrink and crack. After the well cementation set cement added with the expanding agent material provided by the invention is cured for 24 hours and solidified under the condition of 60 ℃ (clear water), the volume shrinkage of the set cement is smaller and basically kept stable, which indicates that the volume shrinkage of the well cementation set cement is compensated by adding the expanding agent and the crack resistance of the well cementation set cement is ensured.
Claims (9)
1. A preparation method of an oil well cement expanding agent sequentially comprises the following steps:
s1, grinding dolomite, calcium stearate and magnesium stearate by a ball mill, stirring, and mixing with diatomite;
s2, drying and tabletting the mixed materials in sequence to obtain test pieces;
s3, pre-sintering the test piece, cooling and crushing to obtain powder;
s4, calcining the powder at a high temperature, and quenching after keeping the temperature for a period of time to obtain an expanding agent block;
and S5, grinding the expanding agent block by using a ball mill to obtain the cement expanding agent.
2. The method for preparing an oil well cement expansive agent according to claim 1, wherein in the step S1, the dolomite, the calcium stearate and the magnesium stearate are ground by a ball mill, the average particle size is 1500-3200 meshes, the ground magnesium stearate and the calcium stearate are added into the ground dolomite for stirring, the stirring time is 30-90min, the magnesium stearate and the calcium stearate are mixed with the diatomite, and the mass ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 180-240: 80 to 150:3~8:3~9.
3. The process for producing an oil well cement expansive agent according to claim 2, wherein the dolomite, the calcium stearate and the magnesium stearate have an average particle size of 2500 mesh after grinding.
4. The method for preparing the oil well cement expanding agent according to claim 2, wherein the mass ratio of the diatomite, the dolomite, the calcium stearate and the magnesium stearate is 190-220: 90 to 120:4~6:4~7.
5. The method for preparing an oil well cement swelling agent according to claim 1, wherein in step S2, the drying conditions are as follows: drying at 90 deg.C for 12 hr with box blower; the tabletting conditions were as follows: the pressure is 50 to 65KN, the boosting rate is 0.2KN/s, the pressure is relieved after the pressure is maintained for 185 to 200s, and the pressure is less than or equal to 4.5KN when the pressure is relieved.
6. The method for preparing an oil well cement swelling agent according to claim 1, wherein in step S3, the pre-sintering step is as follows: the temperature is between room temperature and 650 ℃, and the heating time is 35 to 55min; keeping the temperature at 650 ℃ for 5 to 20min; the temperature is raised for 30 to 45min at 650 to 800 ℃; the temperature is increased for 30min at 800-900 ℃, and the heat preservation time is 50-120min.
7. The method for preparing an oil well cement expansive agent according to claim 1, wherein in the step S4, the conditions of the high-temperature calcination are as follows: calcining in a muffle furnace at the temperature of 900-1100 ℃ for 20-35s; the heat preservation time is 30 to 120min; quenching adopts liquid nitrogen quenching mode.
8. The method of claim 1, wherein in step S5, the size of the expansion agent block is 1500-3200 mesh after being ground by a ball mill.
9. The method for preparing an oil well cement swelling agent as claimed in claim 1, 2, 3, 4, 5, 6, 7 or 8, wherein the prepared cement swelling agent is added to oil well cement to obtain well-cementing cement with good gas channeling resistance and crack resistance, and the mass percentage of the cement swelling agent in the oil well cement is 4~5%.
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| 陈平;王红喜;王英;: "一种钢渣基新型膨胀剂的制备及其性能", 桂林工学院学报, no. 02, pages 109 - 112 * |
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