CN111718149A - Oil well cement low-viscosity thixotropic agent and preparation method thereof - Google Patents
Oil well cement low-viscosity thixotropic agent and preparation method thereof Download PDFInfo
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- CN111718149A CN111718149A CN202010736175.4A CN202010736175A CN111718149A CN 111718149 A CN111718149 A CN 111718149A CN 202010736175 A CN202010736175 A CN 202010736175A CN 111718149 A CN111718149 A CN 111718149A
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- thixotropic agent
- cement
- fly ash
- low viscosity
- oil well
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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
- 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
- C04B2103/0085—Thixotropic agents
Abstract
The invention relates to the field of oilfield chemistry and oil-gas well cementing materials, relates to an oil well cement thixotropic agent, and particularly relates to a low-viscosity thixotropic agent suitable for oil well cement and a preparation method thereof. The invention effectively combines the fly ash and the synthetic polymer thixotropic agent, so that the fly ash absorbs the polymer thixotropic agent. The invention utilizes the ball effect of the fly ash to ensure that the cement paste has low viscosity in the pump injection process, and when the cement paste is static, polymers adsorbed on the surface of the fly ash quickly form a grid structure to achieve the thixotropic function. When the polymer is adsorbed on the surface of the fly ash under the action of external force, the grid structure is damaged as long as the fly ash moves under the action of the external force, the thixotropy is broken, and the safe construction in the pump injection process can be effectively ensured.
Description
Technical Field
The invention relates to the field of oilfield chemistry and oil-gas well cementing materials, relates to an oil well cement thixotropic agent, and particularly relates to a low-viscosity thixotropic agent suitable for oil well cement and a preparation method thereof.
Background
The thixotropic cement paste system has good flowing property in the mixing and injection process, and can quickly form a special cement paste system with higher gel strength after the thixotropic cement paste system is static, so that the ideal cement paste thixotropy can effectively solve the problems of leakage and channeling in the well cementation process. At present, thixotropic agents used in thixotropic cement paste systems at home and abroad can be divided into inorganic thixotropic agents and organic thixotropic agents, wherein the inorganic thixotropic agents mainly comprise clay minerals, sulfates, metal carbonates or mixed metal hydroxides and the like, and the organic thixotropic agents mainly comprise cross-linked polymers and synthetic polymers. The cross-linking agent commonly used in the cross-linked polymer thixotropic agent comprises high-valence transition metal ions such as zirconium, yttrium, iron and the like and titanium chelates such as piperyldione, lactic acid, triethanolamine and the like. The synthetic polymers mainly include polymers of acrylamide monomers, and the like.
The thixotropic mechanism is generally considered to be that internal particles or molecules form a network space structure through certain acting force when a liquid is static, the network space structure can be destroyed under the action of external force, macroscopically, the network space structure is static thickened and shear-thinned, and the network space structure is reformed after the external force is removed for a period of time. According to the thixotropic mechanism, most of the prior common thixotropic agents have the side effect of tackifying, and the cement paste is difficult to pump due to overlarge viscosity, so that an oil well cement low-viscosity thixotropic agent needs to be researched, and the thixotropic agent has certain engineering significance for narrow annulus or small pipe grouting.
Disclosure of Invention
The invention mainly aims to provide a low-viscosity thixotropic agent for oil well cement, and a cement paste system prepared by adopting a conventional water-solid ratio has low viscosity and strong thixotropic property after the thixotropic agent is added.
In order to achieve the purpose, the invention adopts the following technical scheme:
a low viscosity thixotropic agent for cement is prepared from powdered coal ash and synthetic polymer as thixotropic agent.
Optionally, the synthetic polymer thixotropic agent is formed by polymerizing 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) and Acrylamide (AM), and the proportion of the thixotropic agent is (3-4) to (7-6).
Optionally, the crosslinking agent is N, N-Methylene Bisacrylamide (MBA), and the addition amount of the crosslinking agent is 0.5-3% of the mass of the monomer.
Optionally, the initiator is ammonium persulfate, and the addition amount of the initiator is 1-4% of the mass of the monomer.
The optional fly ash has the particle size of 200-500 meshes, and the addition amount of the fly ash is 900 percent of the mass of the monomer.
Wherein the mass of the monomer is the sum of the mass of two monomers, namely 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) and Acrylamide (AM).
The invention also provides a preparation method of the cement low-viscosity thixotropic agent, which comprises the following steps:
(1) adding the fly ash into a synthetic polymer thixotropic agent solvent,
(2) stirring to form slurry;
(3) heating the slurry to make the fly ash adsorb and synthesize the polymer thixotropic agent;
(4) drying to obtain the product.
Optionally, the synthesized polymer thixotropic agent solvent in the step (1) is prepared by the following method: 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), Acrylamide (AM) and N, N-Methylenebisacrylamide (MBA) are dissolved in water to form a solution, and ammonium persulfate is added to the solution to form a solution.
Optionally, the heating in the step (3) is performed at 75 ℃ for 2 hours.
The invention further provides a cement paste system comprising a cement paste and the cement low-viscosity thixotropic agent. The cement slurry is prepared at a conventional water-to-solid ratio, such as 0.44.
Specifically, the method comprises the following steps: the invention provides an oil well cement low-viscosity thixotropic agent, which is prepared by the following steps:
2-acrylamido-2-methylpropanesulfonic Acid (AMPS), Acrylamide (AM) and N, N-Methylenebisacrylamide (MBA) were dissolved in water to form a solution, and ammonium persulfate was added to the solution to form a solution I. And adding a certain amount of fly ash into the solution I, and uniformly stirring to form slurry I. And (3) reacting the slurry I for 2h at 75 ℃. Then drying and crushing to obtain the product.
The mass ratio of the 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) to the Acrylamide (AM) is 3:7-4: 6.
The addition amount of the N, N-Methylene Bisacrylamide (MBA) is 0.5-3% of the mass of the monomer.
The adding amount of the ammonium persulfate is 1-4% of the mass of the monomer.
The mass of water in the solution I is 350-400% of the mass of the monomer.
Preferably, the particle size of the fly ash is 200-500 meshes; the fly ash is divided into F grade and C grade, and if the influence on the cement performance is small, the F grade is mostly used in oil well cement.
The mass of the fly ash in the slurry I is 800-900% of the mass of the monomer.
The oil well cement low-viscosity thixotropic agent disclosed by the invention effectively combines the fly ash and a synthetic polymer thixotropic agent, so that the fly ash adsorbs the polymer thixotropic agent. The invention utilizes the ball effect of the fly ash to ensure that the cement paste has low viscosity in the pump injection process, and when the cement paste is static, polymers adsorbed on the surface of the fly ash quickly form a grid structure to achieve the thixotropic function. When the polymer is adsorbed on the surface of the fly ash under the action of external force, the grid structure is damaged as long as the fly ash moves under the action of the external force, the thixotropy is broken, and the safe construction in the pump injection process can be effectively ensured.
Drawings
FIG. 1 is a micrograph of a low viscosity thixotropic agent.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1 oil well Cement Low viscosity thixotropic agent
The thixotropic agent is prepared from the following components by the following method:
3 parts AMPS, 7 parts AM and 0.1 part MBA are dissolved in 32 parts water to form a solution, and then 0.1 part ammonium persulfate is added to the solution to form solution I. And adding 80 parts of fly ash into the solution I, and uniformly stirring to form slurry I. And (3) reacting the slurry I for 2h at 75 ℃. Then drying and crushing to obtain a product A as shown in figure 1.
Example 2 oil well Cement Low viscosity thixotropic agent
The thixotropic agent is prepared from the following components by the following method:
4 parts AMPS, 6 parts AM and 0.2 part MBA are dissolved in 36 parts water to form a solution, and then 0.2 part ammonium persulfate is added to the solution to form solution I. And adding 90 parts of fly ash into the solution I, and uniformly stirring to form slurry I. And (3) reacting the slurry I for 2h at 75 ℃. Then drying and crushing to obtain a product B.
Example 3 oil well Cement Low viscosity thixotropic agent
The thixotropic agent is prepared from the following components by the following method:
3 parts AMPS, 7 parts AM and 0.3 part MBA are dissolved in 40 parts water to form a solution, and then 0.3 part ammonium persulfate is added to the solution to form solution I. And adding 80 parts of fly ash into the solution I, and uniformly stirring to form slurry I. And (3) reacting the slurry I for 2h at 75 ℃. And then drying and crushing to obtain a product C.
Example 4A Low viscosity thixotropic agent for oil well Cement
The thixotropic agent is prepared from the following components by the following method:
4 parts AMPS, 6 parts AM and 0.3 part MBA are dissolved in 44 parts water to form a solution, and then 0.4 part ammonium persulfate is added to the solution to form solution I. And adding 90 parts of fly ash into the solution I, and uniformly stirring to form slurry I. And (3) reacting the slurry I for 2h at 75 ℃. And then drying and crushing to obtain a product D.
The preparation method of the cement paste comprises the following steps:
100 parts of grade G oil well cement and 8 parts of low viscosity thixotropic agent are dry mixed, a water-cement ratio of 0.44 is adopted, and then the cement paste is prepared according to GB/T10238-2015 standard. The prepared cement paste is respectively CA、CB、CC、CD
The slurry thixotropy testing method comprises the following steps:
after the cement slurry is prepared according to the GB/T19139-2012 oil well cement test method, the reading of phi 3 is recorded as R when the six-speed rotational viscometer is used for testing for 10s, and then the reading of phi 3 is recorded as R1 when the slurry is placed for 10 min. The greater R1 is greater than R, the better the thixotropy of the slurry.
Comparative example 1
Aiming at the currently common inorganic thixotropic agent, fumed silica A200 is selected for carrying out thixotropy test, and the performance parameters are shown in Table 1.
TABLE 1 fumed silica A200 Performance parameters
The preparation method of the cement paste comprises the following steps:
100 parts of grade G oil well cement and 1 part of fumed silica A200 are dry blended, using a water-cement ratio of 0.44, and the slurry is then formulated according to GB/T10238-2015 standard. The prepared cement paste is respectively CE
Comparative example 2
Aiming at the organic thixotropic agent commonly used at present, xanthan gum is selected for carrying out thixotropy test, and the performance parameters are shown in table 2.
Table 2 xanthan gum performance parameters
The preparation method of the cement paste comprises the following steps:
100 parts of grade G oil well cement and 1 part of xanthan gum are dry mixed, a water cement ratio of 0.44 is adopted, and then the cement paste is prepared according to GB/T10238-2015 standard. The prepared cement paste is respectively CF
Thixotropic properties were measured as shown in Table 3, and the test temperature was 60 ℃.
Table 3.
| Sample(s) | Φ600 | Φ300 | Φ200 | Φ100 | Φ6 | Φ3 | Φ3(10s) | Φ3(10min) |
| CA | 230 | 135 | 84 | 66 | 21 | 18 | 19 | 76 |
| CB | 205 | 124 | 76 | 64 | 20 | 19 | 20 | 83 |
| CC | 226 | 140 | 88 | 58 | 21 | 18 | 20 | 73 |
| CD | 215 | 132 | 79 | 66 | 20 | 19 | 21 | 85 |
| CE | Over-range | 278 | 205 | 194 | 30 | 23 | 23 | 37 |
| CF | Over-range | Over-range | 235 | 204 | 67 | 56 | 60 | 75 |
As can be seen from the test results in the table, both comparative thixotropic agents were selected to have significant thickening properties.
As can be seen from Table 3, the slurries according to examples 1 to 4 of the invention have low viscosity and strongly thixotropic properties, while comparative examples 1 and 2 have marked thickening properties.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A low viscosity thixotropic agent for cement is prepared from powdered coal ash and synthetic polymer as thixotropic agent.
2. The cement low-viscosity thixotropic agent according to claim 1, wherein the synthetic polymer thixotropic agent is formed by polymerizing 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) and Acrylamide (AM) in a ratio of (3-4) to (7-6).
3. A cement low viscosity thixotropic agent according to claim 2 wherein the crosslinking agent is N, N-Methylene Bisacrylamide (MBA) added in an amount of 0.5 to 3% by mass of the monomers.
4. The cement low viscosity thixotropic agent of claim 2 wherein the initiator is ammonium persulfate added in an amount of 1-4% by mass of the monomer.
5. The cement low viscosity thixotropic agent as claimed in claim 2, wherein the fly ash has a particle size of 200-500 mesh and is added in an amount of 800-900% by mass based on the mass of the monomer.
6. A method of making a cement low viscosity thixotropic agent as claimed in any one of claims 1 to 5, characterised in that it comprises the steps of:
(5) adding the fly ash into a synthetic polymer thixotropic agent solvent,
(6) stirring to form slurry;
(7) heating the slurry to make the fly ash adsorb and synthesize the polymer thixotropic agent;
(8) drying to obtain the product.
7. The method for preparing a low-viscosity thixotropic agent for cement according to claim 6, wherein the synthetic polymer-based thixotropic agent solvent of the step (1) is prepared by: 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), Acrylamide (AM) and N, N-Methylenebisacrylamide (MBA) are dissolved in water to form a solution, and ammonium persulfate is added to the solution to form a solution.
8. The method for preparing a cement low viscosity thixotropic agent according to claim 7, wherein the heating in the step (3) is performed at 75 ℃ for 2 hours.
9. A cement slurry system comprising a cement slurry and the cementitious low viscosity thixotropic agent of any one of claims 1-5.
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